Download Service Manual Alltech Model 3300 ELSD

Grace Davison Discovery Sciences
Service Manual
Alltech® Model 3300 ELSD
Manual Part No. 3300100SM
8/15/2007
Important Safety Guidelines for the Model 3300 ELSD
Please read the following cautions and warning statements carefully before using the Model 3300
ELSD:
•
Warning: The equipment must be used as specified by the manufacturer
otherwise overall safety will be impaired.
•
Warning: All service must be completed by qualified personnel only.
•
Warning: Only use the power supply cord recommended by the manufacturer.
•
(
•
Warning: Fire hazard, only use the same type and rated CERTIFIED fuse
250V 5A F).
Warning: Shock hazard, disconnect power before replacing the fuse.
•
Warning: Remove power cord from the power module to disconnect electrical
power from the unit.
•
Warning: Check the MSDS forms and dispense and dispose of all reagents in
accordance with local and national regulations.
•
Warning: Be sure to provide proper ventilation for all solvent vapors.
•
Warning: Avoid open flames and sparks when using flammable solvents.
•
Warning: If the unit is damaged and does not function properly, stop the unit
safely and contact the manufacturer immediately.
•
Warning: Class 3B LASER radiation inside can cause severe eye damage. Do not
open or defeat interlocks. Avoid exposure to the beam.
ii
Table of Contents
1. Introduction ......................................................................................................................... 4
1.1 About the Model 3300 ELSD ...................................................................................................................... 4
1.2 Principle of Operation ................................................................................................................................ 5
2. Installation ........................................................................................................................... 6
2.1 What You Will Need .................................................................................................................................... 6
2.2 Unpacking.................................................................................................................................................... 6
2.3 Controls and Features................................................................................................................................ 7
2.3.1 Front Panel....................................................................................................................................... 7
2.3.2 Back Panel ...................................................................................................................................... 8
2.4 Making Electrical and Fluid Connections................................................................................................. 9
3. Navigating the Software Interface.................................................................................... 10
3.1 Main Screen............................................................................................................................................... 10
3.2 Operation ................................................................................................................................................... 10
3.2.1 Mode ............................................................................................................................................... 10
3.2.2 Start/Stop Run ............................................................................................................................... 11
3.2.3 Lock/Unlock Detector.................................................................................................................... 11
3.2.4 Chart ............................................................................................................................................... 11
3.2.5 Autozero ......................................................................................................................................... 12
3.3 Method ....................................................................................................................................................... 12
3.3.1 New ................................................................................................................................................. 12
3.3.2 Open................................................................................................................................................ 13
3.3.3 Edit .................................................................................................................................................. 13
3.3.4 Delete .............................................................................................................................................. 14
3.3.5 Wizard ............................................................................................................................................. 14
3.4 Configuration ............................................................................................................................................ 14
3.4.1 Alarm............................................................................................................................................... 14
3.4.2 Serial Number ................................................................................................................................ 15
3.4.3 Outputs ........................................................................................................................................... 15
3.4.4 Display............................................................................................................................................ 15
3.4.5 Heaters............................................................................................................................................ 15
3.4.6 Date and Time ................................................................................................................................ 16
3.4.7 Language........................................................................................................................................ 16
3.4.8 Pressure Units ............................................................................................................................... 16
3.4.9 Network .......................................................................................................................................... 16
3.4.10 Timed Mode Changes ................................................................................................................... 16
i
3.5 Maintenance .............................................................................................................................................. 17
3.5.1 Manual Control .............................................................................................................................. 17
3.5.2 Logs ................................................................................................................................................ 18
3.5.3 Tests ............................................................................................................................................... 18
3.5.4 Files................................................................................................................................................. 18
3.5.5 Service Tech .................................................................................................................................. 19
3.5.6 Calibration...................................................................................................................................... 19
3.5.7 About .............................................................................................................................................. 19
4. Routine Operation ............................................................................................................. 20
4.1 Safety ......................................................................................................................................................... 20
4.2 Operating Notes ........................................................................................................................................ 20
4.3 Selecting Initial Operating Conditions.................................................................................................... 20
4.4 Startup Sequence ..................................................................................................................................... 20
4.5 Shutdown Sequence................................................................................................................................. 21
4.6 Optimization Procedure ........................................................................................................................... 21
5. Maintenance....................................................................................................................... 22
5.1 Cleaning Mode .......................................................................................................................................... 22
5.2 Nebulizer Cleaning Procedure................................................................................................................. 22
5.3 Drift Tube Cleaning Procedure................................................................................................................ 23
5.4 Optics Cleaning Procedures.................................................................................................................... 24
5.4.1 Optics Block Cleaning Procedure ............................................................................................... 24
5.4.2 Laser Window Cleaning Procedure ............................................................................................. 25
5.4.3 Photodiode Cleaning Procedure.................................................................................................. 25
5.4.4 Pre-Amp Lens Assembly Cleaning Procedure........................................................................... 26
5.5 Fuse Replacement .................................................................................................................................... 30
6. Diagnostics and Troubleshooting ................................................................................... 31
6.1 Errors ......................................................................................................................................................... 31
6.2 Performing Diagnostic Tests................................................................................................................... 34
6.2.1 Nebulizer Gas Pressure Test........................................................................................................ 34
6.2.2 Gas Flow Test ................................................................................................................................ 35
6.2.3 Optics Test ..................................................................................................................................... 36
6.2.4 Optics Heating Test....................................................................................................................... 37
6.2.5 Heater Stability Test ...................................................................................................................... 38
6.2.6 Power Supply Test ........................................................................................................................ 39
6.3 Diagnosing Baseline Noise...................................................................................................................... 40
6.4 Troubleshooting Charts ........................................................................................................................... 41
6.5 Software Troubleshooting Procedure .................................................................................................... 44
ii
7. Appendix ............................................................................................................................ 45
7.1 Specifications............................................................................................................................................ 45
7.2 Contact Information.................................................................................................................................. 45
7.3 Replacement Parts.................................................................................................................................... 46
7.4 Service Kit ................................................................................................................................................ 46
7.5 Software Upgrade Procedures ................................................................................................................ 47
7.5.1 Complete Software Re-Installation Procedure ........................................................................... 47
7.5.1.1 FPGA Installation Procedure........................................................................................... 47
7.5.1.2 LOLO Upgrade Procedure ............................................................................................... 49
7.5.1.3 WinCE OS Initial Setup Procedure.................................................................................. 50
7.5.1.4 Application Initial Setup Procedure................................................................................ 52
7.5.2 Pen Drive Software Upgrade Procedure ..................................................................................... 54
7.6 Calibration Procedures ............................................................................................................................ 56
7.6.1 Heater Calibration.......................................................................................................................... 56
7.6.2 Gas Flow Calibration..................................................................................................................... 58
7.6.3 Laser/Preamp Calibration............................................................................................................. 59
7.7 Schematics ................................................................................................................................................ 60
7.7.1 Electronic Schematic .................................................................................................................... 60
7.7.2 Gas Flow Path................................................................................................................................ 61
7.8 Heaters, RTDs, and Thermofuses ........................................................................................................... 62
7.8.1 Checking the Heaters, RTDs, and Thermofuses ........................................................................ 62
7.8.1.1 Checking the Heaters ...................................................................................................... 62
7.8.1.2 Checking the RTDs.......................................................................................................... 62
7.8.1.3 Checking the Thermofuses ............................................................................................ 63
7.8.2 Heater, RTD, and Thermofuse Replacement Procedures ......................................................... 63
7.8.2.1 Heater Replacement Procedure ...................................................................................... 63
7.8.2.2 RTD Replacement Procedure.......................................................................................... 64
7.8.2.3 Thermofuse Replacement Procedure............................................................................. 65
7.9 Model 3300 ELSD QC Procedure............................................................................................................. 66
7.10 Volatile Mobile Phase Modifiers ............................................................................................................. 67
7.11 Warranty, Returns, and Repairs ............................................................................................................. 68
7.12 Useful References.................................................................................................................................... 69
iii
1. INTRODUCTION
1.1 ABOUT THE MODEL 3300 ELSD
The Alltech Model 3300 ELSD is designed for use with High
Performance Liquid Chromatography (HPLC) systems to
analyze any sample compound that has sufficiently lower
volatility than the mobile phase. Some of its possible
application areas include carbohydrates, pharmaceuticals,
lipids, triglycerides, underivitized fatty and amino acids,
polymers, surfactants, nutraceuticals, and combinatorial
libraries.
Evaporative light scattering detection eliminates common
problems associated with other HPLC detectors. Refractive
Index (RI) detectors can be complicated by solvent front
interferences, baseline instability, and gradient incompatibility.
RI detectors can also have a less sensitive response than
ELSD. Low-wavelength UV can suffer baseline drift with steep
gradients and also requires that the analyte contains a
chromophore. ELSD does not have these limitations. It can
achieve stable baselines with multisolvent gradients for
improved resolution and faster separations. Also, since ELSD
response does not depend on the sample’s optical
characteristics, the sample does not require a chromophore or
fluorophore for detection.
The Model 3300 ELSD features the most advanced
evaporative light scattering detection technology available. It
provides sensitivity in the low nanogram range. An intuitive,
Windows-based software interface provides a nested menu
of options for detector operation, including Method Wizard for
simplified method development, multiple languages, and builtin Diagnostic tests for troubleshooting. The Model 3300 ELSD
also features compact, stackable dimensions, allowing it to fit
easily into limited laboratory space.
4
Lower mobile phase flow rates will require lower gas flow rates
for optimal nebulization. Substitution of a 2.1mm ID column for
your standard 4.6mm ID column will allow you to greatly
reduce the mobile phase flow rate while also increasing the
sensitivity of the analysis.
1.2 PRINCIPLE OF OPERATION
The unique detection principle of evaporative light scattering
detection involves a three-step process: nebulization of the
column effluent to form an aerosol, solvent evaporation within
a heated drift tube, and detection of the non-volatile solute
particles in the light scattering cell.
EVAPORATION
Evaporation of the volatile components in the aerosol occurs
in a heated, stainless steel drift tube. The optimum drift tube
temperature setting for an application will depend on mobile
phase composition, mobile phase flow rate, and on sample
volatility. Highly organic mobile phases require lower drift
tube temperatures for evaporation than highly aqueous
mobile phases. Lower mobile phase flow rates require lower
drift tube temperatures than higher mobile phase flow rates.
Semi-volatile analytes require the use of much lower drift tube
temperatures to obtain optimum sensitivity. The optimum
temperature should be determined by observing the signal-tonoise ratio with respect to temperature.
NEBULIZATION
Within the Model 3300 ELSD drift tube, a PTFE-coated,
stainless steel impactor plate is located three inches from the
nebulizer. The plate is perpendicular to the aerosol path so
as the aerosol contacts the plate, larger droplets exit through
the drain tube on the side panel. The remaining droplets pass
around the impactor and travel through the drift tube to the
optical cell for detection. The removal of the larger droplets
allows operation of the Model 3300 ELSD at low
temperatures, making it ideal for the analysis of semi-volatile
compounds.
EVAPORATION
Non-volatile impurities in the mobile phase or nebulizing gas
will produce noise. Using the highest quality gas, solvents,
and volatile buffers (preferably filtered) will greatly reduce
baseline noise. Noise will also increase if the mobile phase
has not been completely evaporated. Detector settings must
be carefully selected to ensure adequate mobile phase
evaporation.
DETECTION
DETECTION
The non-volatile sample particles emerge from the drift tube
in the mobile phase vapor and enter the light scattering cell.
In the optical cell, sample particles scatter light emitted by a
laser light source. The scattered light is detected by a silicon
photodiode, generating a signal proportional to sample mass.
This signal is sent to the analog output for data collection.
The advanced design of the Model 3300 ELSD optical
1
components provides excellent sensitivity for HPLC analysis.
1
NEBULIZATION
The column effluent from an HPLC separation enters the
nebulizer, where it is mixed with a steady stream of nebulizing
gas (usually nitrogen) to form an aerosol. The aerosol consists
of a uniform distribution of droplets whose size is dependent
on the gas flow rate used for the analysis. The lower the gas
flow rate used, the larger the resulting droplets will be. Larger
droplets scatter more light and increase the sensitivity of the
analysis, but they are also more difficult to evaporate in the
drift tube. There will be an optimum gas flow rate for each
method which will produce the highest signal-to-noise ratio.
5
US Patent #6229605; other patents pending
2.2 UNPACKING
2. INSTALLATION
The Model 3300 ELSD detector and its accessories are
shipped in the same container. Unpack components carefully,
making sure all items in the list below have been included
and are in good condition. Save the container and packing
material for future use.
2.1 WHAT YOU WILL NEED
In addition to the Model 3300 ELSD detector and its
accessories, the following will be needed for installation of a
complete chromatographic system:
The Model 3300 ELSD shipping container should contain the
following:
Exhaust System:
• A fume hood or other ventilation device located close
to the detector to remove the detector exhaust from
the laboratory.
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
NOTE: Make sure the exhaust system provides
adequate but not excessive suction.
Excessive suction can cause a noisy
baseline.
Gas Supply:
• A supply of clean, dry nebulization gas, preferably
nitrogen, regulated from 65 to 80 psig. 99.9% purity or
better is recommended. The gas source can be a highpressure gas cylinder, high-pressure liquid tank, or a
nitrogen generator.
HPLC System Components:
• An HPLC pump, isocratic or gradient, capable of
low-pulsation solvent delivery at a flow rate ranging
from at least 0.1 to 1.5mL/min against pressures of
at least 3,000 psig. Lower flow rate capabilities may
be necessary for smaller bore columns.
Model 3300 ELSD
Model 3300 ELSD Operating Manual
Model 3300 ELSD Performance Documents
Model 3300 ELSD Driver for Agilent ChemStation CD*
Power Cord
Signal Cable
PEEK Tubing: 1/16" OD x .005" ID, 10’
SofGrip Fittings, 10/pk
Gas Tubing, 10’
Gas Fittings: 1/8” Brass Nut and Ferrule
Drain Tubing, 5’ (Reservoir not included)
Drain Tubing Clamp
Exhaust Adaptor
Exhaust Tubing, 20’
14-Pin Connector
Open-End Wrench, 3/8" x 7/16"
Open-End Wrench, 1/4" x 5/16"
Hex Ball Driver, 3/32" x 5 1/4”
Hex Ball Driver, 7/64" x 4”
Drift Tube Cleaning Brush
Fuse, 5 Amp
*The 3300 ELSD Driver for Agilent ChemStation CD can be
used with Agilent ChemStation to control and collect data
from the 3300 ELSD.
Agilent ChemStation must be
purchased separately.
• An autosampler or manual injection valve.
• A column capable of separating the compounds of
interest. If you are uncertain which column to use,
contact your Grace Davison Discovery Sciences
representative or the Grace Technical Support Group for
assistance (Phone: 1-800-33-SOLVE).
The Model 3300 ELSD has been carefully shipped to ensure
that it is received in proper condition. Any damage to the
container or its contents should be reported immediately to
your local distributor or to Grace Davison Discovery Sciences.
Please refer to Section 7.11, Warranty, Returns, and Repairs,
for more information.
• A guard column or cartridge compatible with the
separation column is recommended to prolong
separation column lifetime.
• A column heater, if needed.
Refer to Section 7.3, Replacement Parts, for part numbers if
replacement parts are needed.
• A data system or integrator, capable of accepting
analog voltage data. 0 -10mV or 0 -1000mV systems
can be used.
Other:
• HPLC-grade mobile phase solvents.
NOTE: Only volatile buffers may be used in the
mobile phase. Refer to Section 7.10,
Volatile Mobile Phase Modifiers, for a list of
suitable buffers.
• Solvent reservoirs, tubing, inlet filters, paper, etc.
required for pump and data system operation. Consult
the appropriate manuals for requirements.
6
2.3 CONTROLS AND FEATURES
1
9
2
4
5
7
6
8
3
Figure 2.1: Front Panel of 3300 ELSD; Door Removed
7. Nebulizer Gas Tubing: The gas tubing carries nitrogen
gas to the nebulizer gas inlet.
2.3.1 FRONT PANEL (FIGURE 2.1)
1. LCD (Liquid Crystal Display): The LCD displays the
software interface screens.
2. Soft Power Button: The Model 3300 ELSD can be
powered on/off from the front panel of the unit using the
soft power button. NOTE: The power button on the back
panel must be set to the On position in order for the front
panel button to be active.
8. Drain Port: The DRAIN port is located on the right side of
the front panel. The drain tubing and clamp included with
the unit are connected to the DRAIN port and then directed
to a waste reservoir (not included) located at bench level if
the unit is stacked or floor level. NOTE: The drain tubing
must not be submerged in the liquid inside the reservoir
during operation.
3. Liquid Inlet: The column effluent tubing connects to the
LIQUID INLET with a 1/16" male fitting.
9. Keypad: The keypad is used to interact with the software
interface screens.
4. Nebulizer Liquid Tubing: The stainless steel tubing
carries the column effluent to the liquid inlet of the
nebulizer.
10. Removable Door (not shown): The front door can be
opened or removed to access the nebulizer and drift tube
for cleaning. To remove the door, gently pull the door
towards you.
5. Impactor Cartridge: The cartridge can be removed in
order to access the drift tube for cleaning. Refer to Section
5.3, Drift Tube Cleaning Procedure, for details.
6. Nebulizer: The column effluent and nitrogen gas are
combined within the nebulizer to form an aerosol. The
nebulizer is easily removed for cleaning by pushing in and
using a counterclockwise twisting motion.
7
2.3.2 BACK PANEL (FIGURE 2.2)
1
8
2
3
7
4
5
9
6
10
Figure 2.2: Model 3300 ELSD Back Panel
7. Exhaust Outlet: Nebulizer gas, mobile phase vapor, and
solute mist or particles produced during an analysis will exit
the detector through the EXHAUST outlet. The exhaust
outlet accepts the exhaust adaptor and exhaust tubing
included with the unit, which must be then directed to a
fume hood.
1. Signal Output: The signal cable included with the unit is
connected to the SIGNAL OUTPUT port on the back panel
of the unit and is used to send the analog signal to the data
collection device.
2. RS-232: This port is currently reserved for service tech
functions only.
8. Fan: Provides cooling airflow through the instrument. Do
not block.
3. USB Host: A pen drive (not included) can be inserted into
this port for file importing/exporting and software upgrades.
9. Power Module: The power module contains a socket for
the incoming power cord. It also contains the main power
switch, which is used to turn the system power On/Off, and
the line fuse. The module is autoselecting for 85-265V and
contains a 5 Amp fuse.
4. USB Device: This port is currently reserved for service
tech functions only.
5. Ethernet: This port can be used with the 3300 ELSD
Driver for Agilent ChemStation. This port is also used for
service tech functions
10. Gas Inlet: The GAS INLET accepts the nebulizer gas
supply tubing. The inlet features a quick-connect port,
which requires no additional fittings. Gas pressure should
be regulated from 65 – 80psi.
6. 14-Pin Connector: Outputs TTL/contact closure signals or
accepts signals from peripheral equipment.
8
External Output: Pin 9: Normally Open (NO) (+)
Pin 10: Common (-)
Pin 11: Normally Closed (NC) (+)
2.4 MAKING ELECTRICAL AND FLUID
CONNECTIONS
1. Unpacking the Unit: Remove the ELSD from its
shipping container and position it on a level surface near
the column outlet of your HPLC system and the fume
hood. Make sure there is free flow of air to the bottom of
the ELSD and to the cooling fan at the back panel of the
ELSD. Allow the detector to warm to ambient
temperature if necessary. Save the shipping container
for future use.
Pins 9, 10, and 11 on the Model 3300 ELSD can output
a TTL/contact closure signal to other instruments.
Consult the appropriate manuals for wiring details.
Fault Relay: Pin 12: Normally Open (NO) (+)
Pin 13: Common (-)
Pin 14: Normally Closed (NC) (+)
Pins 12, 13, and 14 on the Model 3300 ELSD can
output a TTL/contact closure signal to stop pump flow
when an error occurs on the detector. Consult the
appropriate manuals for wiring details.
2. Exhaust Adaptor: Screw in the threaded exhaust
adaptor provided in the accessory kit to the EXHAUST
port on the back panel of the unit.
3. Fill the Internal Drain Reservoir: Place a beaker under
the DRAIN port on the right side panel. Using a water
bottle or pipette, add water into the EXHAUST port on
the back panel of the unit until excess liquid is seen
exiting the DRAIN port. Filling the internal drain reservoir
prevents gas from escaping the drift tube.
4. Power Connection: Plug the power cord provided with
the unit into the power module on the back panel of the
detector. The module is autoselecting for 85-265V.
WARNING: Only use the power supply cord
recommended by the
manufacturer.
6.
Gas Connection: Connect the nitrogen gas supply
tubing to the GAS INLET on the back panel. The
nitrogen gas supply should be regulated from 65 – 80
psig. A stable gas flow and pressure are necessary for
reproducible results.
The gas must be free of
contaminants, such as oil, water, particulates, or any
other non-volatile substances. A 0.1um gas filter is
built into the instrument.
7.
Liquid Connection: Connect the column effluent line
to the LIQUID INLET with a 1/16" male fitting. The ID
and length of the tubing between the column and the
detector should be kept as small as possible to avoid
band broadening. 0.005" ID tubing is recommended for
best results. Tubing and fittings are included in the
ELSD 3300 accessory kit.
8. Drain Setup: Attach the drain tubing and clamp
included with the detector to the DRAIN OUTLET on the
right side of the front panel. Extend the tubing to a drain
waste container (not included) either at bench level if
the detector is stacked or at floor level. Make sure the
container is sealed to prevent solvent fumes from
escaping. Monitor the liquid level in the container during
operation and decant excess liquid when the level
approaches the top of the container. CAUTION: Do
NOT allow the tubing to become submerged in the
liquid inside the container. Remember that the waste
container will contain solvents from your mobile phase
and should be disposed of properly.
5. 14-Pin Connector: Insert the 14-pin connector into the
port on the back panel. Make the appropriate wiring
connections to the 14-pin connector depending on which
of the following functions are needed:
Start: Pin 1: Ground (-) Pin 2: Signal (+)
Pins 1 and 2 on the Model 3300 ELSD can accept a
TTL/contact closure signal to start a method run on the
detector.
Standby: Pin 3: Ground (-) Pin 4: Signal (+)
Pins 3 and 4 on the Model 3300 ELSD can accept a
TTL/contact closure signal to put the detector into
Standby mode.
9. Signal Output: Connect the signal cable provided with
the unit to the SIGNAL OUTPUT port on the back panel
of the detector and connect to your data collection
device.
Gas Shutoff: Pin 5: Ground (-) Pin 6: Signal (+)
Pins 5 and 6 on the Model 3300 ELSD can accept a
TTL/contact closure signal to turn off gas flow at the end
of a run. This signal is typically sent from an autosampler
or a data collection system. Consult the appropriate
manuals for wiring information.
10. Exhaust Tubing:
Connect the exhaust tubing
included with the unit to the EXHAUST outlet on the
rear panel of the unit. Extend the tubing to the
hood/ventilation system. There should be no low spots
in the tubing where condensate can collect.
Autozero: Pin 7: Ground (-) Pin 8: Signal (+)
Pins 7 and 8 on the Model 3300 ELSD can accept a
TTL/contact closure signal from a start signal cable to
autozero the detector. This signal is typically sent from
an autosampler or a manual injection valve with a
position-sensing switch. Consult the appropriate manuals
for wiring information.
NOTE: Make sure the exhaust system provides
adequate but not excessive suction.
Excessive suction can cause a noisy
baseline.
9
Mode status until the equilibration requirements are met.
The equilibration requirements are: lower drift tube, upper
drift tube, and optics block must be within 1.5°C of their set
points; gas flow must be within 0.3L/min of its set point; the
temperatures and gas flow must meet the requirements for
60 seconds before the message disappears.
3. NAVIGATING THE SOFTWARE
INTERFACE
The Model 3300 software interface features a collapsible
menu located in the upper left corner of the LCD screen. The
following sections describe the software menu options in
detail. The Help Button, “?” can be pressed in many software
screens in order to access Help Screens which offer
assistance with using the software functions.
• Timed Mode Change Reminder (not shown): If a timed
mode change has been scheduled, a reminder for the
event will be displayed next to the Mode status.
3.1 MAIN SCREEN
• Errors: Any errors that occur on the instrument will be
displayed in the lower right corner of the screen.
The software Menu is located in the upper left corner of the
screen. There are four main Menu headers: Operation,
Method, Configuration, and Maintenance.
The following
sections describe the software functions within these headers.
3.2 OPERATION
3.2.1 MODE
The Model 3300 ELSD has four operational modes: Standby,
Run, Heating, and Cleaning.
The Operation screen is the main screen displayed during use
of the instrument. This screen provides the following
information for the currently loaded method:
STANDBY MODE
• Method Name: Currently loaded method name.
• Temperature: Set point and read value of the drift tube
temperature in °C. The temperature range is from 25.0 to
o
120.0 C. NOTE: There are two heated zones in the drift
tube, a lower zone and an upper zone. The value displayed
on the main screen is the average value for the two zones.
The individual values are displayed in the Manual Control
screen (see Section 3.5.1 for details).
• Gas Flow: Set point and read value of the nebulizer gas
flow rate in L/min. The gas flow range is from 0.0 to
4.0L/min.
Select Operation/Mode/Standby using the arrows on the
keypad and press Enter to put the detector into Standby mode.
In Standby mode, the heaters, gas flow, and laser are off. The
signal output is not displayed, and the chromatogram trace is
not active. The detector enters Standby mode after power-up
with the last saved method conditions.
• Gain: Current gain setting. Possible gain values are 1, 2,
4, 8, and 16. A gain setting of 1 produces an unamplified
signal, and each increase in gain setting produces twofold
signal amplification over the previous setting.
RUN MODE
• Signal Output: The signal output in mV is displayed when
the instrument is in Run or Cleaning modes. The output is
not displayed in Standby or Heating modes. If the output
value exceeds 2.5V, the signal output will read ‘High’. If
output drops below -500mV, the signal output will read
‘Low’.
• Method Run Time: The elapsed time for the method run
is displayed in the upper right corner if a method run has
been started. The time value will remain until the method
run has been stopped.
• Chart: The chromatogram trace of up to 60 minutes will be
active for Run and Cleaning modes.
Select Operation/Mode/Run using the arrows on the keypad
and press Enter to put the detector into Run mode. In Run
mode, the heaters, gas flow, and laser are on. The signal
output is displayed and the chromatogram trace is active. Run
mode is used for sample analysis.
• Mode: The current mode of the detector is displayed
(Standby, Run, Heating, or Cleaning).
• Equilibrating Indicator: If the detector is in Run mode
and the heaters and gas flow have not reached their set
points, the screen will display “Equilibrating” next to the
10
HEATING MODE
3.2.3 LOCK/UNLOCK DETECTOR
The Lock Detector option can be used to lock the method
settings on the detector to prevent unwanted method changes
during operation.
Select Operation/Mode/Heating using the arrows on the
keypad and press Enter to put the detector into Heating mode.
In Heating mode, the heaters are on, but the gas flow and
laser are off. The signal output is not displayed and the
chromatogram trace is not active. Heating mode keeps the
detector in a ready state, so the user won’t have to wait for
temperature equilibration when switching to Run mode for
sample analysis.
Select Operation/Lock Detector using the arrows on the
keypad and press Enter to reach the Lock Detector screen.
Enter and then re-enter the PIN using the keypad. Press
Accept to lock the detector, or press Cancel to cancel locking
the detector.
CLEANING MODE
To unlock the detector, select Operation/Unlock Detector and
press Enter to bring up the Unlock Detector screen. Enter the
PIN created when the detector was locked to unlock the
detector. The detector can also be unlocked by recycling the
power on the unit.
Select Operation/Mode/Cleaning using the arrows on the
keypad and press Enter to put the detector into Cleaning
mode. In Cleaning mode, the heaters, gas flow, and laser are
o
on. Temperature is set to 110 C, gas flow is set to 2.0L/min,
and Gain is set to 1. The detector should be run with 100%
water or other suitable solvent at 1.0mL/min for at least one
hour to clean the detector. Cleaning mode can be used for
routine cleaning of the detector to prevent any buildup of
sample materials inside the drift tube and optics. A dirty drift
tube and optics can cause excess baseline noise.
3.2.4 CHART
The Chart displays a scalable chromatogram trace of up to 60
minutes.
ZOOM
3.2.2 START/STOP RUN
The Zoom function can be used to zoom in/out on the
chromatogram trace. Select Operation/Chart/Zoom using the
arrows on the keypad and press Enter. The zoom tool will
then appear in the lower left corner of the screen.
Select Operation/Start Run using the arrows on the keypad
and press Enter to manually start a method run. The method
elapsed time will then appear in the upper right corner of the
screen above the output, and the timed events programmed in
the method will start. This function should be used only if
timed events will be used with the method.
Select
Operation/Stop Run and press Enter to manually stop the
method run. Refer to Section 3.3.1 for more information on
programming timed method events. Alternately, method timed
events can be started by connecting the proper wiring to the
Start input pins on the back panel of the unit. Refer to Section
2.4 for details.
11
Use the up arrow to Zoom out the Y-axis; use the down arrow
to Zoom in the Y-axis; use the left arrow to zoom in the X-axis;
or use the right arrow to zoom out the x-axis. Once the
desired chart view has been achieved, press Accept to save
the new chart view, or press Cancel to return to the original
chart view. The x-axis range is –60 to 0 minutes. The y-axis
range is –500mV to 2.5V. To reach Pan directly from Zoom,
press Enter.
ENABLE/DISABLE Y-AXIS AUTOSCALE
PAN
RESET SCALE
The Pan function can be used to pan left, right, up, or down on
the chromatogram trace. Select Operation/Chart/Pan using
the arrows on the keypad and press Enter. The Pan tool will
then appear in the lower left corner of the screen:
The Reset Scale function will zoom out the chart view to its
maximum x-axis and y-axis values: -60 to 0 min; -500mV to
2.5V. Select Operation/Chart/Reset Scale using the arrows
on the keypad and press Enter to reset the chart axes.
The Enable Y-Axis Autoscale function causes the chart to
automatically scale to the highest peak and ensures that the
chromatogram trace will always be on-scale.
Select
Operation/Chart/Enable Y-Axis Autoscale and press Enter to
enable this feature. Select Operation/Chart/Disable Y-Axis
Autoscale and press Enter to disable this feature.
3.2.5 AUTOZERO
The Autozero function can be used to zero the output on the
detector. To autozero, select Operation/Autozero using the
arrows on the keypad and press Enter. The autozero value will
depend on the full-scale voltage setting on the detector. For a
1V full-scale voltage setting, the default Autozero value is
5mV. For a 10mV full-scale voltage setting, the default
Autozero value is 0mV. If the Custom Autozero Output has
been enabled, the detector will be autozeroed to the value
selected, from 0 to 100mV. Refer to Section 3.4.3 for more
details on setting the Custom Autozero Output value.
Use the up arrow to Pan up the Chart; use the down arrow to
Pan down the Chart; use the left arrow to Pan left on the
Chart; or use the right arrow to Pan right on the Chart. Once
the desired chart view has been achieved, press Accept to
save the new chart view, or press Cancel to return to the
original chart view. The x-axis range is –60 to 0 minutes. The
y-axis range is –500mV to 2.5V. To go directly to Zoom from
Pan, press Enter.
3.3 METHOD
Methods are created to set the temperature, gas flow, gain,
and event settings on the detector.
3.3.1 NEW
USER DEFINED SCALE
Select Method/New using the arrows on the keypad and press
Enter to bring up the New Method window:
The User Defined Scale screen can be used to enter user
defined x-axis and y-axis values for the chart scaling. Select
Operation/Chart/User Defined Scale using the arrows on the
keypad and press Enter to reach the User Defined Scale
screen:
Enter the Method Name, Temperature, Gas Flow, Gain, and
Timed Events using the keypad. Use the up/down arrows to
tab through the method parameters.
Enter the minimum and maximum x-axis and y-axis values in
the window that appears. The x-axis range is –60 to 0
minutes. The y-axis range is –500mV to 2.5V. Once the new
chart values have been entered, press Accept to save the new
chart settings or press Cancel to return to the original settings.
Method Name: The Method Name may include the following
characters: A - Z, a - z, 1 - 9, <space>, or . (period). Rapidly
press a button on the keypad to cycle between letter and
number options. For upper case, press Shift and then enter
the letter.
12
Temperature: Enter a temperature value between 25 -120oC
using the keypad.
DELETE EVENT
Gas Flow: Enter a value between 0.0 – 4.0L/min using the
keypad.
To Delete an event, use the up/down arrows to highlight the
event to be deleted from the table. Then use the right arrow
and the down arrow to select Delete, and press Enter. The
event will then be deleted.
Gain: Enter a value of 1, 2, 4, 8, or 16 using the keypad. Each
increase in gain setting will produce twofold signal
amplification over the previous setting.
Once all method parameters have been entered, press Accept
to save the new method. The Save Method window will then
appear:
Events: Events can be added to the method in order to
program timed gain changes or timed external output events.
Timed gain changes can be used so sample compounds of
widely varying concentration can be on-scale in the same
chromatogram. Timed external output events can be used to
trigger events on other instruments.
NEW EVENT
To add a new timed event, use the up/down arrows to highlight
the New button and press Enter. The New Event window will
then appear:
Use the up/down arrows or the keypad to select a method
number for the new method. Press Accept to save the new
method, or press Cancel to cancel the new method.
3.3.2 OPEN
Select Method/Open using the arrows on the keypad and
press Enter to open an existing method. The Open Method
window will then appear:
Enter the Event Time, from 0 – 60 minutes. Enter the Event
Type (Change Gain or Set Control Relay). If Change Gain has
been selected, then enter the Gain value: 1, 2, 4, 8, or 16. If
Set Control Relay has been selected, select On or Off for the
External Contact. Once the new event has been created,
press Accept to save the new event, or press Cancel to cancel
the new event.
EDIT EVENT
Use the up/down arrows or enter the method number on the
keypad to select a method from the list. Press Accept and the
method will then load on the main screen, or press Cancel to
cancel loading the method.
To Edit an existing event, use the up/down arrows to highlight
the event to be edited from the table. Then use the right arrow
to select Edit and press Enter. The Edit Event table will then
appear:
3.3.3 EDIT
To Edit an existing method, select Method/Edit using the
arrows on the keypad and press Enter. The Edit Method
window will then appear:
Make the desired changes to the Event Time, Event Type,
Gain, or External Contact. Press Accept to save the event
changes, or press Cancel to cancel the changes.
13
Mobile Phase Flow Rate
Select the Mobile Phase flow rate using the left/right arrows.
Possible choices are 0.2, 0.5, 1.0, 2.0, and 3.0mL/min. Press
Continue to continue on to the next Method Wizard screen, or
press Cancel to cancel the Method Wizard.
Use the up/down arrows to tab through the method
parameters and enter a new Method Name, Temperature, Gas
Flow, Gain, and/or Events using the keypad. Press Accept to
save the new method settings, or press Cancel to return to the
original method settings.
3.3.4 DELETE
To Delete a method, select Method/Delete and press Enter.
The Delete Method window will then appear:
Sample Concentration
Use the left/right arrows to select the sample concentration
from the list. Press Continue to reach the next Method Wizard
screen, or press Cancel to cancel using the Method Wizard.
Select a method to delete from the list using the up/down
arrows or by entering/cycling a number. Press Accept to
delete the method, or press Cancel to cancel deleting the
method.
3.3.5 WIZARD
The Method Wizard can help provide initial detector settings
based on the mobile phase solvent composition, mobile phase
flow rate, and sample concentration. Select Method/Wizard
and press Enter, and the first Method Wizard screen will
appear:
Finished
The final screen in the Method Wizard provides the
recommended Temperature, Gas Flow, and Gain settings
based on the mobile phase solvent composition, mobile phase
flow rate, and sample concentration. Press Finish to continue
creating the method, and the New Method window will appear,
or press Cancel to cancel the Method Wizard.
3.4 CONFIGURATION
3.4.1 ALARM
The Alarm function can be used to sound an alarm when
errors occur on the detector. Select Configuration/Alarm using
the arrows on the keypad and press Enter to bring up the
Alarm Configuration window:
Select Mobile Phase Solvents
Use the left/right arrow keys to select from the list of solvents.
Use the up/down arrows to tab down the table. Enter a
percentage for each solvent. The total percentage must add
up to 100%. Once the solvents/percentages have been
entered, press Continue to continue on to the next screen in
the Method Wizard, or press Cancel to cancel using the
Method Wizard.
14
Use the left/right arrows to select Enabled or Disabled. If
Enabled, the alarm will sound when errors occur on the unit
and will continue to sound until the errors are remedied. If
Disabled, the alarm will not sound when errors occur on the
unit. Press Accept to save the alarm configuration, or press
Cancel to return to the original alarm configuration.
CUSTOM AUTOZERO
Use the left/right arrows to select Enabled or Disabled for the
Custom Autozero. If Enabled, the user can select an Autozero
Offset, from 0 – 100mV. If Disabled, the Autozero will be
based on the full-scale voltage setting on the detector: 5mV
for 1V FS; 0mV for 10mV FS.
3.4.2 SERIAL NUMBER
AUTOZERO OFFSET
If the Custom Autozero has been enabled, enter a value from
0 – 100mV for the Autozero offset. This is the signal output
that will be displayed when the detector is autozeroed. If the
Custom Autozero has been disabled, then the Autozero Offset
will be grayed out. Press Accept to save the changes to the
Outputs Configuration, or press Cancel to cancel the changes.
*This function is available in Service Tech Mode only.
To configure the serial number on the detector, first enter
Service Tech mode by selecting Maintenance/Service Tech
using the arrows on the keypad and press Enter. Enter “atat”
for the Service Tech password and then press Accept. Once
in Service Tech mode, select Configuration/Serial Number.
The Serial Number Configuration screen will then appear.
3.4.4 DISPLAY
Select Configuration/Display using the arrows on the keypad
and press Enter. The Display Configuration screen will then
appear:
Enter the serial number using the keypad. The serial number
can contain numbers only. Press Accept to save the new
serial number, or press Cancel to cancel the changes. If
Accept is pressed, a Success screen will appear indicating
that the new serial number has been set. Press Accept to
confirm that the new serial number will be saved.
Use the up/down arrows to adjust the Display Contrast. The
up arrow lightens the display, and the down arrow darkens the
display. Press Accept to save the new Display settings and
return to the main screen.
3.4.3 OUTPUTS
3.4.5 HEATERS
Select Configuration/Outputs using the arrows on the keypad
and press Enter. The Outputs Configuration screen will then
appear:
*This function is available in Service Tech Mode only.
To configure the optics block heating % on the detector, first
enter Service Tech mode by selecting Maintenance/Service
Tech using the arrows on the keypad and press Enter. Enter
“atat” for the Service Tech password and then press Accept.
Once in Service Tech mode, select Configuration/Heaters
using the arrows on the keypad and then press Enter. The
Heater Configuration screen will then appear:
FAULT RELAY
Use the left/right arrow keys to select Enabled or Disabled for
the Fault Relay setting. If Enabled, the detector will output a
signal to stop a pump if errors occur on the unit. The proper
wiring must be connected for the Fault Relay to work. Refer to
Section 2.4 for wiring details. If Disabled, errors will not trigger
an output to a pump for pump shutdown.
Enter a value for the Optics Heating % in the blank provided.
The default value is 90%. The Optics Block will heat to this %
of the Drift Tube temperature setting. Press Accept to save
the new Heater setting, or press Cancel to cancel the
changes.
FULL-SCALE VOLTAGE
Use the left/right arrows to select 10mV or 1V for the full-scale
voltage, depending on your data collection system.
15
3.4.6 DATE AND TIME
3.4.8 PRESSURE UNITS
Select Configuration/Date and Time using the arrows on the
keypad and press Enter. The Date and Time Configuration
screen will then appear:
Select Configuration/Pressure Units using the arrows on the
keypad and press Enter. The Pressure Units Configuration
screen will then appear:
Enter the Date (month, day, and year) and the Time (hour,
minute, and second) using the keypad. Use the up/down
arrows to tab across the entry blanks. Select the Time Zone
from the list using the left/right arrows. Press Accept to save
the new date and time configuration, or press Cancel to cancel
the changes.
Select Bar or Psi and the new pressure unit setting will take
effect.
3.4.9
NETWORK
To configure the Ethernet port on the back panel of the
detector, first connect an Ethernet cable between the Ethernet
port and a PC. Then select Configuration/Network using the
arrows on the keypad and press Enter.
The Network
Configuration window will then appear:
3.4.7 LANGUAGE
The Model 3300 ELSD can be configured for the following
languages: English, Spanish, French, German, Italian,
Chinese (Simplified), Korean, and Japanese. The detector
must contain the proper software versions in order to be
compatible with certain languages; consult Grace Discovery
Sciences for further details. Select Configuration/Language
using the arrows on the keypad and press Enter. The
Language Configuration screen will then appear:
Use the left/right arrows to select DHCP Enabled or Disabled.
If Disabled is selected, enter the IP address, Subnet Mask,
and Gateway settings. If Enabled is selected, the IP address,
Subnet Mask, and Gateway will be grayed out and should fill in
automatically once the connection is made. Press Accept to
save the new settings, or press Cancel to cancel the new
settings.
Use the up/down arrows to select a language from the list.
Press Accept to save the new language configuration, or press
Cancel to cancel the new language configuration. If Accept
has been entered, the Restart Device screen will then appear:
3.4.10 TIMED MODE CHANGES
Timed Mode Change Events can be used to put the detector
into another operation mode using a timer. This can be
convenient to schedule routine cleaning, heating, etc. events.
A reminder for the next Timed Mode Change will be displayed
on the main screen next to the Mode.
NEW TIMED MODE CHANGE
Select Configuration/Timed Mode Changes/New using the
arrows on the keypad and press Enter to bring up the New
Timed Mode Change Event window:
The unit must be restarted before the language change can
take effect. Select Yes to restart the device and change the
language, or select No and the new language will take effect
the next time the unit is rebooted.
16
Select an Event Type from the list using the left/right arrows
keys: Change to Standby mode, Change to Heating mode,
Change to Run mode, or Change to Cleaning mode. Select
the Recurrence using the left/right arrow keys: Once, Weekly,
or Monthly. For a Recurrence of Once, enter the Day of
Month, Month, Hour, Year, and Minute. Use the up/down
arrows to tab through the entry blanks.
For Weekly
Recurrence, enter the Day of Week, Hour, and Minute. For
Monthly Recurrence, enter the Day of Month, Hour, and
Minute. Press Accept to save the new event settings, or press
Cancel to cancel the new event settings.
Use the up/down arrows to highlight the event to be deleted
from the table. Once the event has been highlighted, press
Accept to delete the selected event, or press Cancel to cancel
deleting the event.
3.5 MAINTENANCE
3.5.1 MANUAL CONTROL
The Manual Control screen can be accessed in order to view
the current status on the detector for laser, gas flow, and
heated zones. Select Maintenance/Manual Control using the
arrows on the keypad and press Enter to reach the Manual
Control screen:
EDIT TIMED MODE CHANGE
To Edit a Timed Mode Change Event, select
Configuration/Timed Mode Changes/Edit using the arrows on
the keypad and press Enter. The Edit Timed Mode Change
Event screen will then appear:
Laser: On/Off
Press 1 to toggle the Laser On or Off. The current signal
output value is displayed in mV.
Use the up/down arrows to select an event from the table.
Press Accept to select the event to be edited, or press Cancel
to cancel the editing. If Accept has been selected, the Edit
Timed Mode Change Event window will appear:
Gas Flow: On/Off
Press 2 to toggle the Gas Flow On or Off. The current gas
flow rate and nebulizer gas pressure are displayed.
Lower Drift Tube: On/Off
Press 3 to toggle the Lower Drift Tube heater On or Off. The
current Lower Drift Tube Temperature value is displayed.
Upper Drift Tube: On/Off
Press 4 to toggle the Upper Drift Tube heater On or Off. The
current Upper Drift Tube Temperature is displayed.
Optics Block: On/Off
Press 5 to toggle the Optics Block heater On or Off. The
current Optics Block temperature is displayed. The Optics
Block heats to 90% of the drift tube temperature set point.
Press Accept to return to the main screen, and the detector
will return to its original settings.
Make the desired changes to the Timed Mode Change Event.
Press Accept to save the changes, or press Cancel to cancel
the changes.
DELETE TIMED MODE CHANGE
Select Maintenance/Timed Mode Changes/Delete using the
arrows on the keypad and press Enter. The Delete Timed
Mode Changes Event screen will then appear:
17
Service Log Entry using the arrows on the keypad and press
Enter. The Create Service Log screen will then appear:
3.5.2 LOGS
VIEW ERROR LOG
Select Maintenance/Logs/View Error Log using the arrows on
the keypad and press Enter. The View Error Log screen will
then appear:
Enter text for the log using the keypad on the front panel or by
connecting a USB keyboard to the back panel. Service Log
entries can contain numbers, letters, and/or symbols. Press
Shift before entering a letter to create an upper case
character. Once the log has been created, press Accept to
save the new Service Log entry, or press Cancel to cancel the
changes.
Each error log entry contains the time of the error, the method
loaded when the error occurred, the mode the detector was in
when the error occurred, and the description of the error. Use
the left/right arrows on the keypad to navigate Error Logs. Use
the up/down arrows to fully view the contents of each log.
3.5.3 TESTS
Diagnostic tests can be run to help troubleshoot the unit. The
available tests are:
VIEW SERVICE LOG
*This function is available in Service Tech Mode only.
•
•
•
•
•
•
To view the Service Logs on the detector, first enter Service
Tech mode by selecting Maintenance/Service Tech/Enter
Service Tech Password using the arrows on the keypad and
press Enter. Enter “atat” for the Service Tech password and
then press Accept. Once in Service Tech mode, select
Maintenance/Logs/View Service Log using the arrows on the
keypad and press Enter. The View Service Log screen will
then appear:
Nebulizer Gas Pressure Test
Gas Flow Test
Optics Test
Optics Heating Test
Heater Stability Test (Service Tech mode only)
Power Supply Test (Service Tech mode only)
To access the diagnostic tests, select Maintenance/
Tests/Nebulizer Gas Pressure Test, Gas Flow Test, Optics
Test, or Optics Heating Test using the arrows on the keypad
and press Enter. To access the Heater Stability Test and the
Power Supply Test, the detector must be in Service Tech
mode first.
To enter Service Tech mode, select
Maintenance/Service Tech/Enter Service Tech Password
using the arrows on the keypad and press Enter. Enter “atat”
for the Service Tech password and then press Accept. Once
in Service Tech mode, select Maintenance/Tests/Heater
Stability Test or Power Supply Test and press Enter.
Refer to Section 6.2 for details on these tests.
Use the left/right arrows on the keypad to navigate through the
Service Logs. Use the up/down arrows to fully view the
contents of each log. Each Service Log contains the time the
log was created, the file and entry number, and the log
information. Service logs contain information on calibration
and configuration changes. Press Accept to exit the Service
Log and return to the main screen.
3.5.4 FILES
Files can be imported or exported from the unit using a pen
drive inserted into the USB Host port on the back panel of the
unit. The USB pen drive must be 128MB or less for the
import/export function to work properly.
EXPORT
CREATE SERVICE LOG ENTRY
To Export files from the detector, insert a pen drive into the
USB Host port on the back panel of the unit. Select
Maintenance/Files/Export/Configuration, Methods, Service Log
(Service Tech mode only), or Error Log using the arrows on
the keypad and press Enter. A message will then appear
indicating that the files have been successfully exported; press
Accept and then the pen drive containing the files can be
removed.
To
enter
Service
Tech
mode,
select
*This function is available in Service Tech Mode only.
To create a Service Log Entry on the detector, first enter
Service Tech mode by selecting Maintenance/Service Tech
using the arrows on the keypad and press Enter. Enter “atat”
for the Service Tech password and then press Accept. Once
in Service Tech mode, select Maintenance/Logs/Create
18
Maintenance/Service Tech using the arrows on the keypad
and press Enter. Enter “atat” for the Service Tech password
and then press Accept.
IMPORT
To Import files to the detector, insert a pen drive containing the
files into the USB Host port on the back panel of the unit.
Select Maintenance/Files/Import/Configuration or Methods and
press Enter. A message will then appear indicating that the
files have been successfully imported; press Accept and the
pen drive can then be removed. The files to be imported must
be located inside a folder named “Alltech” on the pen drive in
order for the import to be successful.
Enter the new password in the blank provided using the
keypad. Press the down arrow to reach the second blank, and
then re-enter the new password. Press Accept to save the
new Service Tech password, or press Cancel to cancel the
changes. If Accept is pressed, a Success screen will then
appear indicating that the Service Tech password has been
changed. Press Accept to confirm the new Service Tech
password.
3.5.5 SERVICE TECH
Service Tech functions are reserved for qualified personnel
only. By entering Service Tech mode, it is possible to access
service functions that cannot be reached in the normal
operation mode.
RESET SERVICE TECH PASSWORD
ENTER SERVICE TECH PASSWORD
To restore the Service Tech password to its default setting
(“atat”), select Maintenance/Service Tech/Reset Service Tech
Password using the arrows on the keypad and then press
Enter. A Success screen will then appear; press Accept to
confirm that the Service Tech password will be restored to its
default setting.
To enter Service Tech mode, select Maintenance/Service
Tech/Enter Service Tech Password using the arrows on the
keypad and press Enter. The Authorize Service Tech screen
will then appear:
3.5.6 CALIBRATION
*This function is available in Service Tech Mode only. To enter
Service Tech mode, select Maintenance/Service Tech/Enter
Service Tech Password using the arrows on the keypad and
press Enter. Enter “atat” as the Service Tech password and
press Accept.
Refer to Section 7.6 for details on the calibration procedures.
3.5.7 ABOUT
Enter the Service Tech password using the keypad, and then
press Accept or Cancel. The default Service Tech password
is “atat”. Once Accept has been pressed, the detector is now
in Service Tech Mode. Service Tech mode provides additional
functions for Configuration and Maintenance: serial number
configuration, optics block heater configuration, calibration,
heater stability and power supply tests, export service log, and
service log.
The About screen displays the current software versions on
the detector and the serial number of the unit. Select
Maintenance/About using the arrows on the keypad and press
Enter. The About screen will then appear:
LOG OUT SERVICE TECH
To log out of Service Tech mode, select Maintenance/Service
Tech/Log Out Service Tech using the arrows on the keypad
and press Enter. The detector will then return to normal
operation mode and Service Tech functions will no longer be
accessible.
Press Accept to return to the main screen.
CHANGE SERVICE TECH PASSWORD
To change the Service Tech password from its default setting
(“atat”), select Maintenance/Service Tech/Change Service
Tech Password using the arrows on the keypad and press
Enter. The Change Service Tech Password screen will then
appear:
19
4.3 SELECTING INITIAL OPERATING CONDITIONS
4. ROUTINE OPERATION
Use the recommendations provided by the Method Wizard for
initial method settings. The Method Wizard can be reached by
selecting Method/Wizard in the software interface. Refer to
Section 3.3.5 for details.
4.1 SAFETY
Please use the following guidelines to insure safe operation of
the Model 3300 ELSD:
1.
Warning: Be sure to provide proper ventilation
for all solvent vapors.
2.
Warning: Use a fume hood or other ventilation
device to prevent the inhalation of any solvent
fumes expelled through the exhaust tube.
3.
Warning: Avoid open flames and sparks when
using flammable solvents.
4.
Warning: Always power off before removing the
cover.
5.
Semi-Volatile Compounds
The recommendations provided by the Method Wizard are
based on non-volatile sample compounds. If the sample
compound is semi-volatile, it may require a lower drift tube
temperature than the Method Wizard recommends. Some
experimentation may be necessary.
Gradient Separations
Choose operating conditions based on the least volatile
portion of the mobile phase when performing gradient
separations.
Unlisted Solvents
For any solvents not listed in the Method Wizard, please refer
to the solvent’s boiling point and vapor pressure in a reference
book such as the Merck Index or Handbook of Chemistry and
Physics. Use the temperature and gas flow rate for the solvent
that most closely matches the boiling point and vapor pressure
of the solvent of interest.
Warning: Laser Radiation – Avoid exposure to
beam – Class IIIB laser.
CLASS 1 LASER PRODUCT
Contains a class 3B 30mW-650nm laser. Designed
to comply with 21CFR 1040.10, 1040.11, and
IEC60825 with amendments as of date of
manufacture.
4.4 STARTUP SEQUENCE
1. Set up the unit as described in Section 2.4, Making
Electrical and Fluid Connections.
No user serviceable components inside. Refer
servicing to qualified personnel.
2. Turn on the nebulizer gas supply.
between 65 and 80 psig.
4.2 OPERATING NOTES
Set the regulator
3. Power up the Model 3300 ELSD.
1. The internal drain reservoir must be filled with liquid (water)
prior to using the detector. The reservoir can be filled
through the EXHAUST port on the back panel. Once water
is visibly draining from the DRAIN port on the right side
panel, the internal drain reservoir has been filled.
4. When the Operation screen appears, set up the desired
method and configuration as indicated in Sections 3.3 and
3.4.
5. Put the detector into Run mode (Operation/Mode/Run).
2. Monitor the liquid level in the drain waste container and
remove excess liquid when necessary. Never let the end
of the drain tubing become submerged in the liquid inside
the container.
6. Allow the detector to equilibrate.
The Equilibrating
indicator will appear next to the Mode in the lower left
corner until the Lower Drift Tube heater, Upper Drift Tube
heater, Optics Block heater, and Gas Flow reach their set
points.
3. Mobile phase should not be flowing when the drift tube is
not at proper vaporization temperature or when the
nebulizer gas is turned off.
7. Once the detector has equilibrated, record a gas-only
baseline for 10-15 minutes. Observe the signal output
displayed on the front panel and on the chromatogram.
You should get a stable, low-noise baseline. The noise
should be in the millivolt range, within 2mV.
4. Only volatile buffers are allowed in the mobile phase. Nonvolatile buffer particles will be viewed as sample by the
detector, causing unwanted baseline noise. Refer to
Section 7.10, Volatile Mobile Phase Modifiers, for a list of
suitable buffers.
8. If the baseline is unstable and/or drifting, the unit may need
longer equilibration time.
9. If the noise is higher than expected, you may want to
perform the optics test to determine if there is a possible
laser or electronics problem. Refer to Section 6.2.3 for
details on the optics test.
20
10. Flush the column with mobile phase before connecting it
to the detector. The length of purging will depend on how
long the column was in storage and what type of sample
and mobile phase were used. It is very important that the
column is free from silica “fines” or other contaminants
before connecting to the ELSD. The Model 3300 ELSD
will detect the contaminants with great sensitivity.
4.6 OPTIMIZATION PROCEDURE
11. After flushing the column, connect it to the LIQUID INLET
on the left side of the front panel on the detector. The
tubing between the column and the nebulizer should be a
short as possible. 0.005” ID tubing is recommended.
12. Turn the pump on to the desired flow rate. Do not exceed
the recommended maximum solvent rates.
13. Check connections for leaks and tighten the fittings, if
necessary.
14. Observe the signal output on the display and the recorded
baseline. After an initial large rise when the pump is
turned on, the signal level should drop close to the “gas
only” level after several minutes. If it remains high after
sufficient equilibration time, the mobile phase may be
contaminated (column fines, buffers, etc.), or the
temperature or gas flow settings may be too low for
optimal evaporation of the mobile phase. Take corrective
measures and allow the system to re-equilibrate for a few
minutes.
15. The detector is ready for sample analysis. The first time
the Model 3300 ELSD is used, you may want to
reproduce the Model 3300 ELSD QC procedure. Refer to
Section 7.9 for details.
4.5 SHUTDOWN SEQUENCE
1.
Turn off the mobile phase flow.
2.
Allow gas only to flow for approximately five minutes to
clear any remaining droplets.
3.
Put the detector in Standby mode
(Operation/Mode/Standby).
4.
Turn off the gas supply at the source, if required.
5.
Power off the ELSD using either the soft power button on
the front panel, or the main power switch on the rear
panel.
NOTE:
•
If the ELSD will not be used for several
days, disconnect the column from the
nebulizer inlet and plug the inlet. Flush the
column before reconnection.
•
Instrument power may be left on when the
instrument is not in use. The laser may be
turned off by putting the detector into
Standby or Heating mode.
21
1.
Set the drift tube temperature, gas flow, and gain to the
initial settings recommended in Section 4.3
2.
Start mobile phase flow and allow the system to
equilibrate.
3.
Increase the drift tube temperature by 1°C increments if
necessary until adequate evaporation of the mobile phase
is achieved (indicated by a stable baseline).
4.
Inject the sample and obtain peak areas for each of the
components. Choose a sample concentration that shows
a peak that is on-scale with baseline noise.
5.
Change the gas flow rate in 0.2L/min increments from the
recommended set point and observe the change in peak
area with each change.
6.
The optimal gas flow rate will produce the largest peaks
with the lowest amount of baseline noise. Plot the signalto-noise ratio vs. peak area to help in identifying the
optimal gas flow rate.
5. MAINTENANCE
5.1 CLEANING MODE
Cleaning mode can be used for routine cleaning of the
detector to prevent any buildup of sample materials inside
the drift tube and optics. A dirty drift tube and optics can
cause excess baseline noise.
To put the detector into Cleaning mode, select
Operation/Mode/Cleaning and press Enter. In Cleaning
mode, the heaters, gas flow, and laser are on. Temperature
is set to 110oC, Gas Flow is set to 2.0L/min, and Gain is set
to 1. The detector should be run with 100% water or other
suitable solvent at 1.0mL/min for at least one hour to clean
the detector. The detector will remain in Cleaning mode
until the detector is switched to another mode.
5.2 NEBULIZER CLEANING PROCEDURE
The nebulizer can become blocked over time with sample and
mobile phase materials. A dirty or blocked nebulizer can cause
increased baseline noise and decreased sensitivity. The
following procedure can be used to clean the nebulizer.
Materials Needed:
•
Open-end wrench, 1/4" x 5/16"
•
HPLC-grade 50:50 methanol:water solution
•
Sonication bath
1.
Power off the unit from the back panel and disconnect the
power cord.
2.
Remove the front door by gently pulling it towards you from
the handle and set aside.
3.
Disconnect the stainless steel liquid inlet line from the
nebulizer using the 1/4” wrench.
4.
Disconnect the quick-connect gas tubing from the front
panel. Push in, then pull out to remove the tubing.
5.
Remove the nebulizer from the drift tube by pushing in and
turning it firmly counterclockwise.
6.
Remove the orange wear band from the nebulizer and set
aside.
7.
Disconnect the nebulizer gas inlet fitting (with gas tubing
attached) from the nebulizer using the 5/16” wrench and set
aside.
8.
Place the nebulizer in
methanol:water solution.
9.
Sonicate the nebulizer in an ultrasonic bath for 10 minutes.
a
beaker
filled
with
50:50
NOTE: Do NOT sonicate the orange wear band, the
nebulizer gas inlet fitting, or the gas tubing.
10. If the nebulizer is still completely blocked, connect a highpressure air line to the nebulizer inlet to help remove the
blockage.
11. If the nebulizer is permanently blocked or cannot be
cleaned, the nebulizer should be replaced.
12. Replace the nebulizer wear band and nebulizer gas inlet
fitting with gas tubing attached.
13. Replace the nebulizer back into the unit by aligning the
grooves and turning clockwise until the nebulizer locks firmly
into place.
14. Reattach the nebulizer gas tubing to the quick-connect
fitting.
15. Reconnect the liquid inlet line to the nebulizer.
16. Replace the front door. The unit is now ready for use.
22
5.3 DRIFT TUBE CLEANING PROCEDURE
CAUTION: The drain hole located on the bottom of
the impactor cartridge must be aligned
with the drain hole inside the unit when
the cartridge is reinserted. Otherwise,
flooding could occur inside the unit.
The drift tube can become dirty over time from sample and
mobile phase materials. A dirty drift tube can cause increased
baseline noise and decreased sensitivity. The following
procedure can be used to clean the drift tube.
Materials Needed:
•
•
•
•
11. Replace the nebulizer back into the unit by aligning the
grooves and turning clockwise until the nebulizer locks
firmly into place.
Open-end wrench, 1/4" x 5/16"
Hex ball driver, 3/32"
Drift tube cleaning brush
HPLC grade water or other suitable cleaning solvent
12. Reattach the nebulizer gas tubing to the quick-connect
fitting.
NOTE: Use only the drift tube cleaning brush
included with the unit. This brush has
been specially selected so it will not travel
too far down the drift tube, which could
splash the optics and result in additional
noise. Do not attempt to force the brush
further into the drift tube than it was
designed to go.
13. Reconnect the liquid inlet line to the nebulizer.
14. Replace the front door. The unit is now ready for use.
1. Power off the unit from the back panel and disconnect the
power cord.
2. Allow the detector to cool for at least 30 minutes.
3. Remove the front door by gently pulling it towards you
from the handle and set aside.
4. Disconnect the stainless steel liquid inlet line from the
nebulizer using the 1/4” wrench.
5. Disconnect the quick-connect gas tubing from the front
panel. Push in, and then pull out to remove the tubing.
6. Remove the nebulizer from the drift tube by pushing in
and turning it firmly counterclockwise. Set the nebulizer
aside.
7. Use the hex ball driver to remove the two screws on the
removable cartridge on the front panel of the unit. Pull out
the cartridge and set aside.
8. Using water or other suitable solvents, wet the drift tube
cleaning brush and carefully insert the brush into the drift
tube from the front panel. NOTE: Use only the cleaning
brush provided with the unit.
9. Carefully clean the sides of the drift tube with the cleaning
brush, loosening any particles that adhere to the drift tube.
10. Once the drift tube has been cleaned, reinsert the
impactor cartridge and tighten the screws. Make sure the
drain hole is located on the bottom of the tube as it is
inserted.
23
9.
5.4 OPTICS CLEANING PROCEDURES
5.4.1 OPTICS BLOCK CLEANING PROCEDURE
The optics block can become dirty over time from sample and
mobile phase materials. Dirty optics can cause increased
baseline noise and decreased sensitivity. The following
procedure can be used to clean the optics block.
With the light trap removed, the optics block can be
accessed for cleaning. Inspect the inside of the optics
block for residue. Swab the inside of the optics block
with a suitable solvent to clean any residue. The
inside of the optics block should be black.
10. Once the optics have been cleaned, reattach the light
trap and replace the 4 hex head screws. Make sure
the light trap has the proper orientation so the
magnetic interlock makes the proper connection.
Refer to Figure 5.1 for details.
WARNING: Use of controls, adjustments, or
performance of procedures other than those
specified herein may result in hazardous exposure
to laser light.
11. Carefully replace the insulation and light trap sweep
gas tubing.
12. Replace the instrument cover and tighten the cover
screws. The unit is now ready for use.
WARNING: Class 3B laser radiation when
optics are open and interlocks defeated. Avoid
exposure to beam.
Materials needed:
•
•
•
•
•
Insulation
Anti-static strap
Phillips screwdriver
Hex ball driver, 3/32"
Suitable cleaning solvent
Cleaning swabs/wipes
Light Trap
Pre-Amp
Board
Magnetic
Interlock
Switch
Laser
Drift Tube
Optics
Block
Reference: Figure 5.1
Sweep Gas Connection
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
Figure 5.1: Optics Block Cleaning
Procedure
2. Power off the unit from the back panel and disconnect the
power cord.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set aside.
CAUTION: The optics block and drift tube may still
be hot.
6. Disconnect the sweep gas tubing from the light trap. The
connection is a quick connect fitting; push in the plastic ring
and then pull the tubing towards you to remove.
7. Remove the insulation from the light trap by gently pulling it
away from the optics block.
8. Using the hex ball driver, remove the 4 hex head screws
connecting the light trap to the optics block and carefully
remove the light trap. Refer to Figure 5.1 for details. To
clean, inspect the inside of the light trap for residue. Swab
the inside of the light trap as necessary with a suitable
solvent to clean any residue. The inside of the light trap
should be black.
24
5.4.3 PHOTODIODE CLEANING PROCEDURE
5.4.2 LASER WINDOW CLEANING PROCEDURE
WARNING: Use of controls, adjustments, or
performance of procedures other than those
specified herein may result in hazardous exposure
to laser light.
WARNING: Use of controls, adjustments, or
performance of procedures other than those
specified herein may result in hazardous exposure
to laser light.
WARNING: Class 3B laser radiation when
optics are open and interlocks defeated. Avoid
exposure to beam.
WARNING: Class 3B laser radiation when
optics are open and interlocks defeated. Avoid
exposure to beam.
Materials Needed:
•
•
•
•
•
Materials Needed:
Anti-static strap
Phillips screwdriver
Hex ball driver, 3/32"
HPLC grade acetone
Cleaning wipes
•
•
•
•
Anti-static strap
Phillips screwdriver
HPLC grade acetone
Cleaning wipes
References: Figure 5.2 and Figure 5.3
References: Figure 5.2 and Figure 5.3
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
2. Power off the unit from the back panel and disconnect the
power cord.
2. Power off the unit from the back panel and disconnect the
power cord.
3. Allow the unit to cool for at least 30 minutes.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws,
1 on each side and 4 on the back panel.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set it aside.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set it aside.
CAUTION: The optics block and drift tube may still
be hot.
CAUTION: The optics block and drift tube may still
be hot.
6. Disconnect the ribbon cable from the preamp board. Allow
it to hang inside the unit.
6. Remove the 4 screws connecting the laser to the optics
mount using the hex ball driver and remove the laser.
Allow the laser to hang inside the unit.
7. Remove the 4 preamp cover screws using the Phillips
screwdriver and remove the preamp cover.
7. Remove the 4 screws on the optics mount using the hex
ball driver and remove the optics mount.
8. Remove the preamp board screws using the Phillips
screwdriver and remove the preamp board.
8. Remove the laser window. Clean the window with acetone
and cleaning wipes until no residue remains.
9. Replace the laser window.
9. Flip the preamp board to access the photodiode sensor.
Use acetone and cleaning wipes to clean the surface of the
photodiode until there is no visible residue.
10. Reattach the optics mount.
10. Replace the preamp board and preamp screws.
11. Reconnect the laser. Make sure the laser is oriented
so the magnetic interlock makes the proper
connection.
11. Replace the preamp cover and preamp cover screws.
12. Reconnect the ribbon cable to the preamp board.
13. Replace the instrument cover and tighten the cover
screws. The unit is now ready for use.
12. Replace the instrument cover and tighten the cover
screws. The unit is now ready for use.
25
13. Carefully replace the lens; make sure the curved surface
faces toward the aperture.
5.4.4 PRE-AMP LENS ASSEMBLY CLEANING
PROCEDURE
14. Replace the 4 screws to the preamp lens assembly.
15. Replace the preamp lens assembly onto the optics block
with the 4 screws.
WARNING: Use of controls, adjustments, or
performance of procedures other than those
specified herein may result in hazardous exposure
to laser light.
16. Replace the preamp mount plate onto the optics block with
the 4 screws.
17. Replace the preamp board and the 4 preamp board
screws.
WARNING: Class 3B laser radiation when
optics are open and interlocks defeated. Avoid
exposure to beam.
18. Replace the preamp board cover and 4 preamp board
cover screws.
19. Reconnect the ribbon cable to the preamp board.
Materials Needed:
•
•
•
•
•
•
20. Replace the instrument cover and tighten the cover
screws. The unit is now ready for use.
Anti-static strap
Phillips screwdriver
Hex ball driver, 3/32”
Hex ball driver, 7/64”
HPLC grade acetone
Cleaning wipes
References: Figure 5.2 and Figure 5.4
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
2. Power off the unit from the back panel and disconnect the
power cord.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set it aside.
CAUTION: The optics block and drift tube may still
be hot.
6. Disconnect the ribbon cable from the preamp board. Allow
it to hang inside the unit.
7. Remove the 4 preamp cover screws using the Phillips
screwdriver and remove the preamp cover.
8. Remove the 4 preamp board screws using the Phillips
screwdriver and remove the preamp board. Set the
preamp board aside.
9. Remove the 4 preamp mount plate screws using the
Phillips screwdriver and remove the preamp mounting
plate.
10. Remove the 4 screws connected to the preamp lens
assembly using the 7/64” hex driver.
11. Flip the preamp lens assembly and remove the 4 screws
using the 3/32” hex driver.
12. Remove the lens and clean with acetone and cleaning
wipes until no fingerprints, smudges, or dirt remain.
26
25
15
14
NOTES:
1. APPLY "CHEMPLEX 1381 HEAT SINK SILICONE" OR SIMILAR TO CARTRIDGE HEATERS WHEN PLACING THEM WITHIN OPTICS BLOCK.
2. CLAMP THERMAL FUSE FROM ITEM 25 TO ITEM 1 USING ITEM 19.
3. MOUNT RESETTABLE THERMAL FUSE FROM ITEM 25 TO ITEM 1 USING ITEM 29.
26
4
13
5
18
9
21
SEE NOTE 1
6
20
10
FIGURE 5.2: OPTICS BLOCK ASSEMBLY
17
28
29
SEE NOTE 3
16
23
24
27
19
SEE NOTE 2
3
1
22
11
7
8
12
2
29
28
27
26
25
0003177
0000216
0000221
0003214
0003218
0003186
0003232
23
24
0001967
22
0003067
0003066
20
21
0003264
0003014
18
19
0003136
17
0003137
15
0002473
0003276
14
16
0003030
13
0003117
0003021
11
12
0003016
0003015
9
10
0002992
0002988
8
7
0003006
0003005
5
6
0002979
0003113
3
4
0002474
2
CM Part #
0002883
1
Item
Number
Title
Ref. Type
Alltech Drawing
Number
Alltech Drawing
Number
Alltech Drawing
Number
McMaster-Carr
#
McMaster-Carr
#
Alltech Drawing
Number
McMaster-Carr
#
McMaster-Carr
#
McMaster-Carr
#
McMaster-Carr
#
Alltech Drawing
Number
McMaster-Carr
#
Alltech Drawing
Number
Alltech Drawing
Number
Alltech Drawing
Number
Alltech Drawing
Number
McMaster-Carr
#
McMaster-Carr
#
Alltech Drawing
Number
Alltech Drawing
Number
McMaster-Carr
#
Alltech Drawing
Number
McMaster-Carr
#
DECIMAL: ±.002"
FRACTIONAL: ± 1/64"
ANGULAR: ±1/2º
GENERAL TOLERANCES
This drawing is the property of Alltech
Associates, Inc. Any reproductions or
modifications of this drawing or its
contents without consent of Alltech is
prohibited.
9431T11
0003014
0003136
92196A109
91793A077
92210A157
92196A150
0003117
92196A113
0003016
0003015
0002992
0002988
0003006
0003005
0002979
9319k147
92196A110
90403A146
91114A007
69965K91
0003214
0003218
91770A146
0003232
91772A153
93405A145
1
1
1
1
1
2
1
4
4
4
1
1
1
2
2
4
4
1
4
1
1
1
1
1
1
1
3
4
1
Quantity
MATERIAL:
DRAWN:
kschmitt
APPROVED: BB
SCALE: 1=1.33 DRAWING NO:
0002882
SIZE D
P/N:
DATE: 09/14/06
REV SHEET
D 1 OF 1
2051 Waukegan Road, Deerfield, IL 60015
(847) 948-8600
Alltech Associates, Inc.
-
-
-
C
C
-
B
-
-
-
-
A
O
-
-
-
-
O
-
D
D
C
B
D
C
B
-
-
C
Revision
DESCRIPTION: Optics Block Assembly
#6-32 x 3/8 L Pan Head
McMaster-Carr
Phillips Screw with Internal
#
Washer
CONFIDENTIAL:
#6 Tooth Lock Washer
Ribbon Cable Clip
Optics Block RTD Wiring
Assembly
Cartridge Heaters and
Thermal Fuse Wiring
Assembly
#6-32 x 3/8" L Truss Head
Phillips Machine Screw
Optics Block Ground Wire
Assembly
#6-32 x 1 L Pan HD Screw
Ref. #
0002883
McMaster- CARR 95345A426
P/N
#6-32 x 5/16 L Pan Head
McMaster-Carr
Phillips Screw with Split Lock #
Washer
#4-40 x 1/4" L Pan Head
Phillips Screw with External
Lock Washer
1/8" Two Channel Metal Strap McMaster-Carr
#
Rubber Disk Light Seal
Optics Block Heater Retainer Alltech Drawing
Number
#4-40 x 7/16" L SHC Screw
#2-56 x 1/4L Binding Head
Slotted Screw
#6-32 x 1 1/2" Flat Head
Socket Cap Screw
#6-32 x 5/8 L SHCS
Magnet Switch Assembly
#4-40 x 3/4" SHC Screw
Pre-amp sheetmetal cover
Pre-Amp mounting plate
assembly
Mounted Laser Assembly
Laser Optic Mount Assembly Alltech Drawing
Number
Pre-Amp Board Assembly
Pre-Amp Optics Assembly
Light Trap Assembly
O-Ring AS568A-024 (1 1/8" ID
x 1 1/4" OD)
#4-40 x 1/2" SHC Screw
Optics Block
NOTES:
11
13
1
3
2
4
12
5
9
10
8
FIGURE 5.3: LASER OPTICS MOUNT ASSEMBLY
7
6
McMaster-Carr #
Alltech Drawing Number
0002487 Optical Window Seal
0002488 Optical Window
0002473 #4-40 x 7/16" L SHC Screw
0003117
0002509 #4-40 SHCS x 5/16 L
0003320 Window Lock Insert
0003321
4
5
6
7
8
9
10
63
DECIMAL: .XX ±.010"; .XXX ±.005"
FRACTIONAL: ± 1/64"
ANGULAR: ±1/2º
UNLESS OTHERWISE SPECIFIED
GENERAL TOLERANCES
This drawing is the property of Alltech
Associates, Inc. Any reproductions or
modifications of this drawing or its
contents without consent of Alltech is
prohibited.
CONFIDENTIAL:
0003020 Male Connector 10-32
Thread to 1/8 Tube Push-In Fitting
Parker #
Alltech Drawing Number
Alltech Drawing Number
McMaster-Carr #
Alltech Drawing Number
MATERIAL:
DRAWN: BY
APPROVED: WM
SCALE: 1 = 1 DRAWING NO:
0002988
SIZE B
P/N:
DATE: 09/14/06
REV SHEET
C 1 OF 1
1
1
1
3
1
4
1
2
1
1
2
1
1
Quantity
Alltech Associates, Inc.
-
B
A
-
O
-
O
-
-
A
-
B
B
Revision
2051 Waukegan Road, Deerfield, IL 60015
(847) 948-8600
68ML-2-0
0002989
0002990
92196A077
0003320
92196A107
0003117
92196A109
45639
0002487
91580A181
0002471
0002472
Ref. #
DESCRIPTION: Laser Optic Mount Assembly
Laser Positioning Spacer
0002989
12
13
0002990 Laser Optic Mount
11
#2-56 x 1/4"L SHCS
Magnet Switch Assembly
McMaster-Carr #
Edmund
Alltech Part Number
McMaster-Carr #
Alltech Drawing Number
0002493 3/4 Retaining Ring
3
Ø1/4 Aperture
0002471
2
Alltech Drawing Number
Ref. Type
0002472 Ø5/16 Aperture
Title
1
Item
CM Part #
Number
NOTES:
1. POSITION CURVE SURFACE OF ITEM 6 TOWARDS ITEM 1.
1
4
3
2
5
FIGURE 5.4: PREAMP LENS BLOCK ASSEMBLY
7
6
0003172
7
CONFIDENTIAL:
#6-32 X 1/2 L Socket
Head Cap Screw
Aspheric Glass Lens
63
DECIMAL: .XX ±.010"; .XXX ±.005"
FRACTIONAL: ± 1/64"
ANGULAR: ±1/2º
UNLESS OTHERWISE SPECIFIED
GENERAL TOLERANCES
This drawing is the property of Alltech
Associates, Inc. Any reproductions or
modifications of this drawing or its
contents without consent of Alltech is
prohibited.
0001997
6
McMaster-Carr #
Melles Griot P/N
McMaster-Carr #
Alltech Drawing Number
McMaster-Carr #
Alltech Drawing Number
Alltech Drawing Number
Ref. Type
4
1
1
1
1
1
1
Quantity
MATERIAL:
DRAWN: BY
APPROVED: WM
SCALE: 1 = 1 DRAWING NO: 0003005
SIZE B
P/N:
DATE: 09/14/06
REV SHEET
C 1 OF 1
Alltech Associates, Inc.
-
-
-
B
-
D
C
Revision
2051 Waukegan Road, Deerfield, IL 60015
(847) 948-8600
92196A148
01-LAG-003
9319k24
0000068
91580A181
0003004
0003003
Ref. #
DESCRIPTION: Pre-Amp Optics Assembly
0000068 .36 ID x .74 OD Aperture
4
AS568A-114 O-Ring
0002493 3/4 Retaining Ring
3
0003135
0003004 Pre-Amp Mount
5
0003003 Lens Mount
1
Title
2
Item
CM Part #
Number
5.5 FUSE REPLACEMENT
WARNING: Only suitably qualified personnel
should carry out these adjustments.
WARNING: Shock hazard, disconnect the
power cord before replacing the
fuse.
WARNING: Fire hazard, only use the same type
and rated CERTIFIED fuse
250V 5A F).
(
1. Power off the detector from the back panel and unplug
the power cord.
2. Gently squeeze the side tabs of the fuse drawer and pull
the fuse drawer straight out. Refer to Figure 5.5 for
details.
3. Remove the blown fuse and replace with the new fuse.
Be sure to use the appropriate fuse: 5 Amp 250V.
Make sure the replacement fuse is placed into the fuse
slot on the right side of the fuse drawer.
4. Replace the fuse drawer. Make sure the fuse inserts into
the fuse slot on the right side of the fuse block. The
correct slot has a metal contact inside the fuse block.
Figure 5.5: Model 3300 ELSD Fuse Block
30
6. DIAGNOSTICS AND TROUBLESHOOTING
6.1 ERRORS
The main screen will list any errors currently occurring on the instrument in the lower right corner. Operation error messages will
remain until the error condition is remedied. Operation errors relate to temperature and gas flow accuracy during operation.
Initialization errors will appear on bootup for 15 seconds and then disappear. Initialization errors relate to calibration issues (i.e.
if the unit is uncalibrated or if the calibration is out of date).
OPERATION ERRORS
ERROR
Drift tube temperature
error.
Optics block temperature
error.
WHEN OCCURS
Drift tube temperature
reading is more than 10°C
(+/-) off its set point.
Optics block temperature
reading is more than 10°C
(+/-) off its set point.
CAUSES
SOLUTIONS
Bad RTD(s).
Check RTD(s). Replace
RTD(s) if bad and then
recalibrate the heaters. Refer
to Sections 7.8 and 7.6.1 for
details.
Bad heater.
Check heater. Replace
heater if bad and then
recalibrate the heaters. Refer
to Sections 7.8 and 7.6.1 for
details.
Bad heater board.
Replace heater board and
then recalibrate the heaters.
Refer to Section 7.6.1 for
details.
Bad processor board.
Replace processor board and
then recalibrate the heaters,
gas flow, and laser/preamp.
Refer to Section 7.6 for
details.
Blown thermofuse.
Allow the resettable fuse 2
hours to reset. Then recheck
the thermofuse and replace if
necessary. Refer to Section
7.8 for details.
Bad RTD.
Check RTD. Replace RTD if
bad and then recalibrate the
heaters. Refer to Sections
7.8 and 7.6.1 for details.
Bad heater(s).
Check heater(s). Replace
heater(s) if bad and then
recalibrate the heaters. Refer to
Sections 7.8 and 7.6.1 for
details.
Bad heater board.
Replace heater board and
then recalibrate the heaters.
Refer to Section 7.6.1 for
details.
31
OPERATION ERRORS (continued)
ERROR
Optics block temperature
error (continued).
Gas flow error.
Inlet gas pressure is low.
WHEN OCCURS
Optics block temperature
reading is more than 10°C
(+/-) off its set point.
Gas flow reading is more
than 0.3L/min (+/-) off its set
point.
Inlet gas pressure is lower
than 40 psig.
CAUSES
SOLUTIONS
Bad processor board.
Replace processor board and
then recalibrate the heaters,
gas flow, and laser/preamp.
Refer to Section 7.6 for
details.
Blown thermofuse.
Allow the resettable fuse 2
hours to reset. Then recheck
the thermofuse and replace if
necessary. Refer to Section
7.8 for details.
Gas source may be low or
empty.
Check gas source and
replace if necessary.
Regulator pressure setting is
too low.
Adjust regulator pressure to
65-80psig.
Nebulizer may be blocked.
Clean nebulizer. Refer to
Section 5.2 for details.
Gas leaks may exist inside
unit.
Check gas flow path for leaks.
Bad gas flow valve and/or
flow meter.
Replace flow meter and/or
valve, and then recalibrate the
gas flow. Refer to Section 7.6.2
for details.
Bad processor board.
Replace processor board and
then recalibrate the heaters,
gas flow, and laser/preamp.
Refer to Section 7.6 for details.
Regulator pressure setting is
too low.
Adjust regulator pressure to
65-80psig.
Gas source may be low or
empty.
Replace gas source if
necessary.
Gas leaks may exist inside
unit.
Check gas flow path for leaks
and remedy.
Bad processor board.
Replace processor board and
then recalibrate the heaters,
gas flow, and laser/preamp.
Refer to Section 7.6 for details.
Bad pressure switch.
Replace pressure switch.
Any errors not included in
this list.
Contact Grace/Alltech.
32
INITIALIZATION ERRORS
ERROR
WHEN OCCURS
CAUSES
SOLUTIONS
The following errors
occurred during
initialization: The device
has not been configured.
Device heater, gas flow,
and/or laser have not been
calibrated. Please contact
a technical service
representative to
recalibrate. Error
encountered while setting
temperature, gas flow, or
gain.
Laser/preamp, gas flow,
and/or heaters have not
been calibrated.
Calibrate the heaters, gas
flow, and/or laser/preamp.
Refer to Section 7.6 for
calibration procedures.
The following errors
occurred during
initialization: Device
heater, gas flow, and/or
laser calibration is out of
date (last calibrated
mm/dd/yyyy hh:mm:ss
AM/PM). Please contact a
technical service to
recalibrate.
Unit requires its yearly
recalibration.
Recalibrate the heaters, gas
flow, and/or laser/preamp as
needed. Refer to Section 7.6
for calibration procedures.
33
6.2 PERFORMING DIAGNOSTIC TESTS
7. Once the test is completed, press Done to return to the
main screen, or press Test to repeat the test.
6.2.1 NEBULIZER GAS PRESSURE TEST
8. If the test has failed, refer to the following table, Nebulizer
Gas Pressure Test Results, for possible fail messages and
their solutions.
1. Make sure the inlet gas pressure is set between 65 and 80
psig before starting the test.
NEBULIZER GAS PRESSURE
TEST RESULTS
2. Turn off mobile phase flow. Wait several minutes for the
detector to stabilize.
3. In the software, select Maintenance/Tests/Nebulizer Gas
Pressure Test and press Enter. The Nebulizer Gas
Pressure Test screen will then appear:
RESULT
Fail: Gas
pressure is
too high.
4. Press Test and the Nebulizer Gas Pressure Test will begin.
The test takes 60 seconds to complete. A timer bar will
appear showing how much time is left for the test:
Fail: Gas
pressure is
too low.
CAUSE
Nebulizer may be
blocked.
Follow the
nebulizer cleaning
procedure in
Section 5.2.
Bad gas pressure
sensor or bad
processor board.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
Gas source may be
low or empty.
Check gas source
and replace if
necessary.
Regulator pressure
may be too low.
Adjust regulator
pressure to 6580psig.
Gas leaks may be
present before the
nebulizer.
Check gas
connections for
leaks and tighten
fittings if
necessary.
Bad gas pressure
sensor or bad
processor board.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
Nebulizer may be
blocked.
Follow the
nebulizer cleaning
procedure in
Section 5.2.
Inlet gas pressure is
unstable.
Check stability of
gas source and
remedy if
necessary.
Gas flow meter or
valve error.
Replace flow meter
and/or valve, and
then recalibrate the
gas flow. Refer to
Section 7.6.2 for
details.
5. The following steps occur during the Nebulizer Gas
Pressure Test:
• Gas flow is set to 2.0L/min and allowed to stabilize.
• Minimum, maximum, and average
pressure values are determined.
nebulizer
gas
• Test results are displayed. The gas flow is returned to its
pre-testing set point.
Fail: Gas
pressure is
unstable.
6. Passing requirements for the Nebulizer Gas Pressure
Test are:
• Nebulizer gas pressure must be between 3 – 30psig.
• Pressure variation must be less than 3 psig during the
testing period.
34
SOLUTION
NEBULIZER GAS PRESSURE
TEST RESULTS (continued)
RESULT
Fail: Gas
pressure is
unstable.
(continued)
CAUSE
Bad gas pressure
sensor or bad
processor board.
SOLUTION
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
6. Passing requirements for the Gas Flow Test are:
• Gas flow must be within 0.2L/min at each gas flow set
point (1.0, 2.0, 3.0, and 4.0L/min).
7. Once the test is completed, press Done to return to the
main screen, or press Test to repeat the test.
6.2.2 GAS FLOW TEST
8. If the test has failed, refer to the following table, Gas Flow
Test Results, for possible fail messages and their solutions.
1. Make sure the inlet gas pressure is set between 65 and
80psig before starting the test.
GAS FLOW TEST RESULTS
2. Turn off mobile phase flow. Wait several minutes for the
detector to stabilize.
RESULT
3. In the software, select Maintenance/Tests/Gas Flow Test
and press Enter. The testing screen will then appear:
CAUSE
Fail: Gas flow is Unstable inlet
unstable.
gas pressure.
SOLUTION
Check stability
of gas source
and remedy if
necessary.
Gas flow meter or Replace flow meter
valve error.
and/or valve, and
then recalibrate the
gas flow. Refer to
Section 7.6.2 for
details.
4. Press Test and the Gas Flow Test will begin. The test
takes 4 minutes to complete. A timer bar will appear
showing how much time is left for the test.
Nebulizer
may need
replacement.
Fail: Gas flow is Gas supply is low
lower than the
or empty.
set point.
Gas supply valve
is closed.
Replace nebulizer.
Check gas supply
and replace if
necessary.
Open gas supply
valve.
Blockage or leaks Check gas line for
in gas line before blockage and leaks;
the detector.
remedy/replace as
necessary.
5. The following steps occur during the Gas Flow Test:
• Gas flow is set to 1.0, 2.0, 3.0, and 4.0L/min and allowed
to stabilize at each flow rate.
• Minimum, maximum, and average gas flow rate values
are determined at each flow rate.
• Test results are displayed. The gas flow is returned to its
pre-testing set point.
35
Gas flow meter
and/or valve
error.
Replace flow meter
and/or valve, and
then recalibrate the
gas flow. Refer to
Section 7.6.2 for
details.
Gas flow
calibration is off.
Recalibrate gas
flow. Refer to
Section 7.6.2 for
details.
• The offset between laser on and laser off, and the
amount of variation in laser signal are determined.
GAS FLOW TEST RESULTS (continued)
RESULT
CAUSE
SOLUTION
Fail: Gas flow
is higher than
the set point.
Gas flow calibration
is off.
Recalibrate gas
flow. Refer to
Section 7.6.2 for
details.
Gas flow meter
and/or valve error.
Replace flow meter
and/or valve, and
then recalibrate the
gas flow. Refer to
Section 7.6.2 for
details.
• Test results are displayed.
6. Passing requirements for the Optics Test are:
• Laser on/off offset must be between 0.5 – 80mV
• Laser off stability must be within 1.5 mV
6.2.3 OPTICS TEST
• Laser on stability must be within 1.5 mV.
1. Make sure the inlet gas pressure is set between 65 and
80psig before starting the test.
7. Once the test is completed, press Done to return to the
main screen, or press Test to repeat the test.
2. Turn off mobile phase flow. Wait several minutes for the
detector to stabilize.
8. If the test has failed, refer to the following table, Optics Test
Results, for possible fail messages and their solutions.
3. In the software, select Maintenance/Tests/Optics Test and
press Enter. The Optics Test screen will then appear:
OPTICS TEST RESULTS
RESULT
CAUSE
Fail: Noise level Bad preamp
at laser off is too board.
high.
4. Press Test and the Optics Test will begin. The test takes
60 seconds to complete. and a timer bar appears indicating
how much time is remaining on the test.
Fail: Offset
between laser
on and laser off
is too high.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section 7.6
for details.
Optics may need
cleaning.
Following the optics
cleaning procedure
in Section 5.4.
Bad preamp
board.
Replace preamp
board and then
recalibrate the
preamp/laser. Refer
to Section 7.6.3 for
details.
Bad processor
board.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section 7.6.
• The laser is turned off and the detector is allowed to
stabilize at Gain 1.
• Minimum, maximum, and average signal data are
recorded for laser on.
36
Replace preamp
board and
recalibrate the
preamp/laser. Refer
to Section 7.6.3.
Bad processor
board.
5. The following steps occur during the test:
• Minimum, maximum, and average signal data are
collected for laser off. The laser is turned on and the
detector is allowed to stabilize.
SOLUTION
OPTICS TEST RESULTS (continued)
RESULT
CAUSE
SOLUTION
Fail: Offset
between laser
on and laser
off is too high.
(continued)
Apertures have
rough edges.
Rotate apertures
o
90 .
Fail: Offset
between laser
on and laser
off is too low.
Laser is not
powering on.
Make sure
interlocks are
activated (including
cover).
Bad laser.
Replace laser and
then recalibrate the
preamp/laser.
Refer to Section
7.6.3 for details.
Bad processor
board.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
Fail: Noise
level at laser
on is too high.
Optics may need
cleaning.
Bad preamp board.
Bad processor
board.
3. Press Test to run the Optics Heating Test. The test takes 1
second to complete. The results screen will then appear.
4. Pass requirements for the test are:
• Optics Block must be 90% (+/-2%) of the Drift Tube
Temperature set point.
5. If the test has failed, refer to the following table, Optics
Heating Test Results for possible causes and solutions.
OPTICS HEATING TEST RESULTS
Following the
optics cleaning
procedure in
Section 5.4.
RESULT
Fail: The Optics
Block
temperature is
xx.x% of the drift
tube
temperature. It
should be
xx.x%.
Replace preamp
board and
recalibrate the
preamp/laser.
Refer to Section
7.6.3 for details.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
6.2.4 OPTICS HEATING TEST
1. The detector must be in Run mode and the heaters
equilibrated before the Optics Heating Test is run.
2. In the software, go to Maintenance/Tests/Optics Heating
Test and press Enter. The testing screen will then appear:
CAUSE
SOLUTION
Detector is in
Standby mode.
Put the detector in
Run mode, allow it
to equilibrate, and
then repeat the test.
Detector is still
equilibrating.
Wait for the detector
to equilibrate and
then repeat the test.
Bad optics block
RTD.
Check RTD(s).
Replace RTD(s) if
bad and then
recalibrate the
heaters. Refer to
Sections 7.8 and
7.6.1 for details.
Bad optics block
heater.
Check heater.
Replace heater if
bad and then
recalibrate the
heaters. Refer to
Sections 7.8 and
7.6.1 for details.
Bad heater board. Replace heater
board and then
recalibrate the
heaters. Refer to
Section 7.6.1.
37
5. The following steps occur during the Heater Stability Test:
OPTICS HEATING TEST RESULTS
(continued)
RESULT
Fail: The
Optics Block
temperature is
xx.x% of the
drift tube
temperature.
It should be
xx.x%.
(continued)
CAUSE
• Minimum, maximum, and average temperature values
for the Lower Drift Tube, Upper Drift Tube, and Optics
Block are determined.
SOLUTION
Bad processor
board.
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section
7.6 for details.
Blown thermofuse.
Allow the
resettable fuse 2
hours to reset.
Then recheck the
thermofuse and
replace if
necessary. Refer
to Section 7.8 for
details.
• Test results are displayed
6. Passing requirements for the Heater Stability Test are:
• Temperature stability for the Lower Drift Tube, Upper
o
Drift, and Optics Block must be within +/- 1 C during the
testing period.
7. If the test has failed, refer to the following table, Heater
Stability Test Results for possible causes and solutions.
8. Once the test is completed, press Done to return to the
main screen, or press Test to repeat the test.
6.2.5 HEATER STABILITY TEST
*This function is available in Service Tech Mode only.
HEATER STABILITY TEST RESULTS
1. Make sure the detector is set to Run mode and is fully
equilibrated before running the test.
RESULT
2. Enter
Service
Tech
mode
by
selecting
Maintenance/Service Tech/Enter Service Tech password
and entering “atat” using the keypad.
Fail (Lower
Drift Tube,
Upper Drift
Tube, and/or
Optics Block)
3. Select Maintenance/Tests/Heater Stability using the arrows
on the keypad and press Enter. The Heater Stability Test
screen will then appear:
CAUSE
Detector is still
equilibrating.
Wait for the
detector to
equilibrate and
then repeat the
test.
Blown thermofuse.
Allow the
resettable fuse 2
hours to reset.
Then recheck the
thermofuse and
replace if
necessary. Refer
to Section 7.8.
Bad RTD(s).
Check RTD(s).
Replace RTD(s)
if bad and then
recalibrate the
heaters. Refer to
Sections 7.8 and
7.6.1 for details.
Bad heater(s).
Check heater.
Replace heater
if bad and then
recalibrate the
heaters. Refer to
Sec. 7.8 & 7.6.1.
4. Press Test and the Heater Stability Test will begin. The test
takes 2 minutes to complete. A timer bar will appear that
shows how much time is left for the test:
38
SOLUTION
HEATER STABILITY TEST RESULTS
(continued)
RESULT
Fail (Lower
Drift Tube,
Upper Drift
Tube, and/or
Optics Block)
(continued)
CAUSE
Bad heater board.
Bad processor
board.
5. Passing requirements for the Power Supply Test are:
• Each voltage value must be +/- 5% of its theoretical
value.
SOLUTION
6. Once the test is completed, press Done to return to the
main screen, or press Test to repeat the test.
Replace heater
board and then
recalibrate the
heaters. Refer to
Section 7.6.1.
7. If the test has failed, refer to the following table, Power
Supply Test for possible fail messages and their solutions.
POWER SUPPLY TEST RESULTS
Replace
processor board
and then
recalibrate the
heaters, gas
flow, and
laser/preamp.
Refer to Section
7.6 for details.
RESULT
Fail.
(1.5, 1.8, 3.3, 4,
5, 12, or -12V)
6.2.6 POWER SUPPLY TEST
*This function is available in Service Tech Mode only.
This test can be run to test the voltages on the processor
board: 1.5V = FPGA Voltage; 1.8V = Card Engine Voltage;
3.3V = Digital Voltage; 4V = Laser Power Supply Voltage; 5V
= Digital Voltage; +12V = Analog Voltage; -12V = Analog
Voltage. Contact Grace/Alltech for more details.
1. Enter
Service
Tech
mode
by
selecting
Maintenance/Service Tech/Enter Service Tech password
and entering “atat” using the keypad.
2. Select Maintenance/Tests/Power Supply Test using the
arrows on the keypad and press Enter. The Power Supply
Test screen will then appear:
3. Press Test and the Power Supply Test will begin. The test
will run until Done is pressed.
4. The results for the test are then displayed. The values are
updated in real-time.
39
CAUSE
Bad processor
board.
SOLUTION
Replace processor
board and then
recalibrate the
heaters, gas flow,
and laser/preamp.
Refer to Section 7.6
for details.
6.3 DIAGNOSING BASELINE NOISE
Start diagnosing the noise at ‘A’ and work down the table until
the source of the baseline noise is determined.
There are many causes for baseline noise. Use the table
below, Diagnosing Baseline Noise, to help identify the source.
DIAGNOSING BASELINE NOISE
SYMPTOM
A. Noise from Column
• Column in-line
• Mobile phase on
• Nebulizing gas on
• Laser on
SOLUTION
1. The column may be leaking silica or packing material.
Replace the column.
Result: Noise disappears when column is removed.
B. Noise from Mobile Phase
• Column removed
• Mobile phase on
• Nebulizing gas on
• Laser on
Result: Noise disappears when pump is stopped.
C. Noise from Gas
• Column removed
• Mobile phase off
• Nebulizing gas on
• Laser on
1. Current drift tube temperature and gas flow rate settings may
not be providing adequate evaporation of the mobile phase.
Re-optimize gas flow and/or drift tube temperature following
the optimization procedure in Section 4.6.
2. The nebulizer, drift tube, and/or optics may be dirty. Refer to
Sections 5.1 – 5.4 for cleaning procedures.
3. The mobile phase may be contaminated with particulate
matter. Filter the current mobile phase or replace it with
freshly prepared and filtered mobile phase.
4. The mobile phase may contain excess air bubbles. Degas
the mobile phase.
5. The pump may be the source. Check pump for pulsations.
Make sure the pump has been sufficiently purged to remove
air. Incorporate a pulse dampener into the system if
necessary. Examine the pump check valve and seals and
replace as necessary.
1. The gas supply may be contaminated with particulates.
Replace with better quality/higher purity gas.
2. The nebulizer, drift tube, and/or optics may need cleaning.
Refer to Sections 5.1 – 5.4 for cleaning procedures.
Result: Noise disappears when gas is turned off.
D. Noise from Flow Optics Block
• Column removed
• Mobile phase off
• Nebulizing gas off
• Laser on
1. The optics may need cleaning. Refer to Section 5.4 for optics
cleaning procedure.
2. Check data cable for noise.
3. Check light trap for condensation. Refer to Section 5.4 for
details on removing the light trap.
Result: Noise disappears when laser is turned off.
E. Noise from Electronics
• Column removed
• Mobile phase off
• Nebulizing gas off
• Laser off
Result: Baseline noise persists under the above conditions.
1. Preamp board is bad. Replace the preamp board and then
recalibrate the preamp/laser. Refer to Section 7.6.3 for
details.
2. Processor board is bad. Replace the processor board and
then recalibrate the heaters, gas flow, and laser/preamp.
Refer to Section 7.6 for details.
40
6.4 TROUBLESHOOTING CHARTS
Consult the following charts to assist in troubleshooting your system:
TROUBLESHOOTING
PROBLEM
CAUSE
SOLUTION
Baseline drift
Detector has not fully equilibrated.
Baseline noise
Follow the procedure in Section 6.3,
Diagnosing Baseline Noise, to
determine the source of the problem
and possible solutions.
Spiking
Drift tube temperature and/or gas flow
rate set too low.
Re-optimize the drift tube temperature and gas
flow rate following the optimization procedure
in Section 4.6.
Gas source contaminated or low
purity.
Use clean, dry, inert gas, usually 99.9% pure
nitrogen.
Mobile phase contaminated or made
of low quality material.
Replace with fresh, filtered, higher-quality
mobile phase.
Nebulizer, drift tube, and/or optical cell
dirty.
Refer to Sections 5.1 – 5.4 for cleaning
procedures.
Improper nebulization.
Nebulizer may be partially obstructed. Refer to
Section 5.2 for nebulizer cleaning procedure.
Thermal fuse(s) may be blown.
Allow the resettable fuses 2 hours to reset. Then
recheck the thermofuse and replace if necessary.
Refer to Section 7.8 for details.
Heater calibration is off.
Recalibrate heaters. Refer to Section 7.6.1 for
details.
Bad RTD(s).
Check RTD(s). Replace RTD(s) if bad and
then recalibrate the heaters. Refer to Sections
7.8 and 7.6.1 for details.
Bad heater.
Check heater. Replace heater if bad and then
recalibrate the heaters. Refer to Sections 7.8
and 7.6.1 for details.
Bad heater board.
Replace heater board and then recalibrate the
heaters. Refer to Section 7.6.1 for details.
Bad processor board.
Replace processor board and then recalibrate
the heaters, gas flow, and laser/preamp. Refer
to Section 7.6 for details.
Thermal fuse may be blown.
Allow the resettable fuses 2 hours to reset. Then
recheck the thermofuse and replace if necessary.
Refer to Section 7.8 for details.
Heater calibration is off.
Recalibrate heaters. Refer to Section 7.6.1 for
details.
Drift tube temperature not
reaching set point
Optics block temperature not
reaching set point
41
Wait for detector to fully equilibrate. Refer to
Section 4.4, Start-Up Sequence, for
equilibration procedure.
TROUBLESHOOTING (continued 1)
PROBLEM
Optics block temperature not
reaching set point (continued)
CAUSE
SOLUTION
Bad RTD(s).
Check RTD(s). Replace RTD(s) if bad
and then recalibrate the heaters. Refer
to Sections 7.8 and 7.6.1 for details.
Bad heater.
Check heater. Replace heater if bad
and then recalibrate the heaters. Refer
to Sections 7.8 and 7.6.1 for details.
Bad heater board.
Replace heater board and then
recalibrate the heaters. Refer to Section
7.6.1 for details.
Bad processor board.
Replace processor board and then
recalibrate the heaters, gas flow, and
laser/preamp. Refer to Section 7.6 for
details.
Gas source valve is closed.
Open gas valve.
Source gas pressure is too low.
Adjust source pressure to 65-80psig.
Gas source may be low or empty.
Replace gas source.
Gas flow meter and/or valve error.
Replace flow meter and/or valve, and then
recalibrate the gas flow. Refer to Section
7.6.2 for details.
Bad pressure switch.
Replace pressure switch.
Bad processor board.
Replace processor board and then
recalibrate the heaters, gas flow, and
laser/preamp. Refer to Section 7.6 for
details.
No power
Blown fuse.
Replace fuse. Refer to Section 5.5, Fuse
Replacement, for details.
No LCD display
Display cable is loose.
Check for loose display cable.
Bad LCD display.
Replace LCD display.
Bad processor board.
Replace processor board and then
recalibrate the heaters, gas flow, and
laser/preamp. Refer to Section 7.6 for
details.
Sample is below the detection limit.
Increase the sample concentration or
injection volume and re-inject.
Sample is volatile at current detector
conditions.
Lower temperature settings are needed for
semi-volatile compounds. Refer to Section
4.6, Optimization Procedure, for details.
Sample is being retained on the
column.
Use a different column for your separation.
Gain is set too low.
Increase the gain value.
No gas flow
No peak(s) detected
42
TROUBLESHOOTING (continued 2)
PROBLEM
No peak(s) detected (continued)
Change in peak height or loss in
sensitivity
Broad peaks
Cut-off peaks
CAUSE
SOLUTION
Autosampler needle is not pulling up
sample properly, or sample loop
blockage.
Repair or replace equipment as needed.
Bad laser.
Replace laser and recalibrate
preamp/laser. Refer to Section 7.6.3 for
details.
Bad preamp board.
Replace preamp board and recalibrate
preamp/laser. Refer to Section 7.6.3.
Bad satellite board.
Replace satellite board.
Bad processor board.
Replace processor board and then
recalibrate the heaters, gas flow, and
laser/preamp. Refer to Section 7.6 for
details.
Nebulizer, drift tube, and/or optics are
dirty.
Clean the nebulizer, drift tube, and optics
as needed. Following the cleaning
procedures in Sections 5.1 – 5.4.
Autosampler needle not pulling up
sample properly, or sample loop
blockage.
Repair or replace equipment as needed.
Bad laser.
Replace laser and recalibrate the
laser/preamp. Refer to Section 7.6.3 for
details.
Bad preamp board.
Replace preamp board and recalibrate
preamp/laser. Refer to Section 7.6.3.
Bad satellite board.
Replace satellite board.
Bad processor board.
Replace processor board and then
recalibrate the heaters, gas flow, and
laser/preamp. Refer to Section 7.6 for
details.
Leak(s) (especially between the column
and detector) present.
Check for loose fittings and tighten if
necessary.
Tubing between column and detector is
too long or too large of an ID.
Use a shorter piece of 0.005 - 0.010" ID
tubing.
Sample concentration too high.
Decrease sample concentration until peaks
are on-scale.
Gain set too high.
Reduce gain value until peaks are onscale.
43
6.5 SOFTWARE TROUBLESHOOTING
PROCEDURE
Use the following procedure to help customers troubleshoot
the software on the 3300 ELSD:
1. Obtain the following information from the customer:
a. A detailed description of the error, including any error
messages displayed on the unit.
b. Serial number of the detector.
c. Software versions on the detector. The software versions
on the detector can be obtained by going to
Maintenance/About on the unit.
d. Configuration, Error Log, and Method files exported from
their unit. These files can be exported by inserting a USB
pen drive (must be 128MB or less; pen drives with greater
than 128MB are not compatible with the 3300 ELSD) into
the USB Host port on the back panel of the unit. Then
select Maintenance/Files/Export in the software to export the
files. The pen drive can then be removed and the files can
be sent via email to Grace/Alltech Technical Support:
[email protected].
e. The information obtained from the customer will then be
forwarded to the Grace/Alltech Engineering department who
will provide further assistance.
44
7. APPENDIX
7.2 CONTACT INFORMATION
7.1 SPECIFICATIONS
Grace Davison Discovery Sciences/
Alltech Associates, Inc.
2051 Waukegan Road
Deerfield, IL 60015 USA
Phone: (847) 948-8600
Fax: (847) 948-1078
Web: www.discoverysciences.com
www.elsd.com*
Technical Support:
1-800-33-SOLVE
[email protected]
Ordering Information: 1-800-ALLTECH
MODEL 3300 ELSD SPECIFICATIONS
Light Source:
Laser diode with collimating
optics, 650nm, max output
less than 30mW, Class IIIB
Product Class:
Class 1 laser product
Detector Element:
Silicon photodiode
Temperature Range:
Ambient to 120°C in 0.1°C
increments
Nebulizer Gas:
Up to 4L/min, nitrogen
preferred, 65psig min.
pressure, 80psig max
pressure
Mobile Phase Flow Rate:
50uL - 3.0mL/min
Analog Outputs:
Selectable for either 0 - 1V or
0 - 10mV full scale
Communications:
Remote Inputs: TTL/Contact
closure-Autozero, Gas
Shutoff, Start, Standby
Outputs: Contact closure-Fault Relay, External Output;
RS232, USB (Device), USB
(Host), Ethernet
Operating Parameter
Selection & Display:
Windows-Based Graphical
LCD with alphanumeric
keypad
Power Requirements:
120/240V, 50/60Hz, 5A
Dimensions:
11.6" H x 10.3" W x 19.5" D
(29.5cm H x 26.2cm W x
49.5cm D)
Weight:
30 lbs (13.6 kg)
Environmental Operating
Temperature:
15 to 40˚C
Relative Humidity:
10 – 90%, Non-Condensing
*Additional information for the 3300 ELSD, including
software updates, can be obtained from the
www.elsd.com website.
45
7.3 REPLACEMENT PARTS
7.4 SERVICE KIT
MODEL 3300 ELSD REPLACEMENT PARTS
Part No.
MODEL 3300 ELSD SERVICE KIT
Qty. Description
5136931
1
2112995
2112993
2107259
2106694
2107268
2112992
2112880
2110773
5126955
2110623
2111502
2111503
2112997
2112990
3112777
2108384
2112994
2112996
N/A
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
3300 ELSD Accessory Kit (includes all
parts listed above the divider)
Signal Cable
Power Cord, 110V
Open-End Wrench, 3/8” x 7/16”
Open-End Wrench, 1/4” x 5/16”
Ball Driver, 3/32”
Ball Driver, 7/64”
Drift Tube Cleaning Brush
PEEK Tubing, 1/16”OD x 0.005”ID, 10’
TM
SofGrip Fittings, 10/pk
Gas Tubing, 10’
1/8” Brass Nut
1/8” Brass Ferrule
Drain Tubing, 5’
Clamp for Drain Tubing
Exhaust Tubing, 20’
Exhaust Adaptor
Fuse, 5 Amp
Model 3300 ELSD Operating Manual
3300 ELSD ChemStation Driver CD
2113967
2113968
2114811
2107480
2107476
2107511
2114472
2114584
2113962
2113961
2113963
2114471
2113960
8606365
2113966
2114652
2114711
2114712
2113943
2114671
2113643
2113956
2113965
2113954
2113964
2113959
2113958
2113952
2113953
2113955
2113957
2113951
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Nebulizer
Nebulizer Wear Band
Nebulizer Chemraz O-Ring
.25 x .79 Aperture
.31 x .74 Aperture
.36 x .74 Aperture
Processor Board
Pre-Amp Assembly (includes sensor)
Display Board
Card Engine Board
Heater Board
Satellite Board
Inverter (for Display Board)
Gas Filter
Optics Block
Thermofuse Complete Assembly
Drift Tube Heater Assembly
Optics Block Heater Assembly
Magnetic Switch Assembly
Gas Pressure Sensor
Membrane Switch Panel
Front Service Door
Nebulizer Cartridge
Inlet Gas Fitting
Impactor
Light Trap
Light Trap Cover
Light Trap Gasket
Light Trap ND Filter
Laser
Power Entry Module
Fuse Drawer
46
Part No.
Qty.
Description
5139415
1
3300 ELSD Service Kit (includes all
parts listed below)
3300100SM
3116580
8617092
3116671
2107799
2113972
2114102
3112023
2113971
2107268
2114101
2113970
2113969
1
1
1
1
1
1
1
1
1
1
1
1
1
3300 ELSD Service Manual
Pre-Amp and Laser Calibration Fixture
Temperature Calibration Box
Drift Tube Temperature Device - Claw
Magnet for Magnetic Switch
128MB Flash Drive
Jumper for Cal Box
SMB Cable
FPGA Cable
3/32” Standard Ball Driver
Small Flat Screwdriver for Pots
Crossover Cable
Serial Modem Cable
7.5 SOFTWARE UPGRADE PROCEDURES
7.5.1.1 FPGA INSTALLATION PROCEDURE
7.5.1 COMPLETE SOFTWARE RE-INSTALLATION
PROCEDURE
Materials Needed:
• Anti-static strap
• Phillips screwdriver
• FPGA cable
• Altera Quartus II programming software (downloaded
onto a pc)
• New FPGA software file (*.pof)
The software re-installation procedure should be completed:
•
•
if the processor board has been replaced
if the existing software files on the unit have
become corrupted.
Reference: Section 7.7.1, Electronic Schematic
These steps must be followed in order for the re-installation
to be successful:
Procedure:
1. Complete the FPGA Installation Procedure in Section
7.5.1.1.
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
2. Complete the LOLO Upgrade Procedure in Section
7.5.1.2.
2. Power off the unit from the back panel and disconnect
the power cord.
3. Complete the WinCE OS Initial Setup Procedure in
Section 7.5.1.3.
3. Using a Phillips screwdriver, remove the cover screws,
1 on each side and 4 on the back panel.
4. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set aside.
4. Complete the Application Initial Setup Procedure in
Section 7.5.1.4.
5. Connect the FPGA cable to connector J14 on the
processor board inside the unit. J14 is a 10-pin
connector located in the lower left corner of the
processor board. The red wire of the FPGA cable
should be towards the back panel of the unit.
6.
Connect the FPGA cable to the parallel port LPT1 on
the PC.
7. Reconnect the power cord and power up the unit.
8. Start the Altera Quartus II Programmer software on the
PC. The following screen will appear:
9. In the Mode drop-down menu at the top of the screen,
select Active Serial Programming:
47
13. In the file name row check the Program/Configuration
and Verify boxes:
10. Click on the Hardware Setup button and select
ByteBlaster (LPT1) from the pull down menu:
14. Press Start in the Altera software and monitor the
Progress bar in the upper right corner:
11. Click on the Add File button and locate the latest
version of the FPGA file on your computer. The file
format should be *.pof:
15. When the Progress bar reaches 100%, power off and
unplug the unit and remove the FPGA cable from J14:
12. Select the file and choose Open.
48
16. Replug in and power up the unit and wait for the main
screen to load.
The output should be:
17. Select Maintenance/About in the software and verify that
the new FPGA version has been loaded.
send update file:
9. On the PC using TeraTerm Pro:
18. If running the complete software re-installation, continue
on in Section 7.5.1.2, LOLO Upgrade Procedure.
Otherwise, the FPGA installation procedure is complete.
a.
Select File->Send File…
b.
Navigate to the directory where the LOLO
upgrade files were placed.
c.
In the Send File dialog box, make sure
that ‘Binary’ is checked under Option.
d.
Doubleclick on the file that has an
extension of .upd to start the download.
e.
In the above image, the name of the file is
7.5.1.2 LOLO UPGRADE PROCEDURE
Materials Needed:
•
•
•
TeraTerm Pro software program (installed on a pc)
Serial cable
LOLO upgrade files
1. Start the TeraTerm Pro software program on the PC.
Select Setup/Serial Port and make sure the settings are:
Baud Rate: 115200, Data: 8 bit, Parity: None, Stop: 1
bit, Flow Control: None, Transmit Delay: 0msec/char
and 0msec/line.
2. Connect the serial cable between the 3300 ELSD and
the PC.
3. Power up the 3300 ELSD while holding down the “q”
character on the PC keyboard. The following should
appear in the serial terminal screen:
*****************************************************************
LogicLoader
(c) Copyright 2002-2005, Logic Product Development, Inc.
All Rights Reserved.
Version 2.0.3-LLH7a404_11 0001
*****************************************************************
1004077_lolo.up
losh> qqqqqqqqqq
10. When the download has completed, LOLO will
automatically update itself. The output should appear
similar to the following:
4. Press Enter to reach the next line in the serial terminal.
5. Run the following command:
info version
................................
erasing flash: 100%
burning flash: 100%
update done.
The response should be similar to the following:
Version : 2.0.3-LLH7a404_11 0001
Build: lpd077 Fri Aug 12 10:08:23 CDT 2005
CPLD_CE_REG_REVISION: 0x32
6.
11. If running the complete software re-installation,
continue on in Section 7.5.1.3, WinCE OS Initial Setup
Procedure. Otherwise, the LOLO installation procedure
is complete.
Examine the version number listed in step 5. If it begins
with 2.0.5 or a larger number, the procedure can be
stopped, no upgrade is necessary. If the version
begins with a number that is less than 2.0.5, continue
with step 7.
7. Install the LOLO upgrade file onto the PC.
8. On the serial terminal run the following command:
update
49
7.5.1.3 WinCE OS INITIAL SETUP PROCEDURE
port. Click OK to accept the dialogs and continue with
step 10 to configure software.
Materials Needed:
•
•
•
•
•
10. After starting, the screen below will appear:
Crossover Ethernet cable
WinCE OS setup files
TeraTerm software (downloaded onto a pc)
Serial cable
Tftpd32.exe software (downloaded onto a pc)
1. Configure a standalone PC with a static IP address. In
these instructions, the IP address of 159.97.84.210 is
used. It doesn’t matter what address is used, but the rest
of the procedure will assume the above address.
NOTE: Make sure this PC is not connected to any other
network. A DHCP server on the PC will be used to
assign an IP address to the ELSD. If this PC is
connected to a network that already has a DHCP server
running, both DHCP servers will be assigning addresses
to PC’s on the network. This will cause corrupting and
confusion on the network.
2. Connect the 3300 ELSD to the PC with a crossover
Ethernet cable.
11. Next Tftpd32 will need to be configured. Click on the
Settings button on the bottom of the window. This will
present a new screen:
3. Copy the OS setup files to a directory on your PC. The
setup files are:
boot.losh
setup.losh
nk.bin
4. Disable any firewall software that may be running on your
PC. If you are unsure how to do this, contact your IS
department. The firewall will most likely interfere with the
DHCP and TFTP Servers.
5. Connect the serial cable to the serial port on the 3300
ELSD and the serial port on the PC.
6. Run TeraTerm Pro to create a serial connection to the
ELSD.
7.
Power up the 3300 ELSD while holding down the q key
on the PC keyboard. This should produce output
similar to the following:
********************************************
LogicLoader
(c) Copyright 2002-2005, Logic Product
Development, Inc.
All Rights Reserved.
Version 2.0.6-LLH7a404_11 0001
********************************************
losh>
12. Configure the settings to match those shown above. Be
sure the IP address matches the IP address on the PC;
in this example the address is 154.97.84.210. Also
make sure to set the base directory to the location
where the OS setup files were saved from step 3 above.
Then click OK to save the settings. If the IP address
was changed, you’ll be prompted to restart the Tftpd32
software, do so now.
8. Run the following command:
ifconfig sm0 up
9. Start the TFTP/DHCP server by launching ‘Tftpd32.exe’.
The first time that Tftpd32 is started, there may be some
error dialogs about not being able to bind the BOOTP
50
b. Create the partition:
13. Next the DHCP server needs to be configured. Click on
the DHCP Server tab and edit the settings to match
those shown below and click the Save button:
add-yaffs app nor 0x00040000 0x01fc0000
The expected output from this command is:
add-yaffs: inserted: start 0x40000 len 0x1fc0000
c. Mount the partition:
mount yaffs /app
The expected output from this command is:
Mounting a YAFFS partition.
--------------------------------------Starting YAFFS file system:
Current YAFFS partition table:
0:
app 00000000 - 0000007e (0)
1:
<NULL>
2:
<NULL>
3:
<NULL>
YAFFS initialized.
---------------------------------------
14. Next the ELSD needs to be configured with an IP
address. Run the following command:
ifconfig sm0 dhcp
15. Once the command returns to the losh prompt, the
machine will have an IP address within a few seconds.
To check the address that was assigned, wait a few
seconds and then run the following command:
17. Next you need to load the OS image and initial boot
files from the TFTP server. The ELSD will need to
know the IP address of the PC running the TFTP
server. The TFTP server displays that information on
its main screen. In the example screen above the IP
address is 159.97.84.210. Replace that address in the
command below with the one from your TFTP server
screen. Do the following sequence of commands:
ifconfig sm0
The expected output from this command is:
sm0: up
100M full-duplex (425)
sm0:mac: 00:08:ee:00:83:77 ip: 159.97.84.10
mask: 255.255.255.0 gw: 159.97.84.210
a. Copy the boot script:
cp/tftp/159.97.84.210:boot.losh/app/boot.losh
In the above output, the IP address assigned to the
ELSD is 159.97.84.10. Write down this address;
it will be needed during the application installation
procedure. If the IP address is all 0’s, wait a few
more seconds and try it again.
The expected output from this command is:
cp /tftp/159.97.84.210:boot.losh ->
/app/boot.losh done
16. Next a YAFFS partition will be created in the flash on
the card engine. This partition will be used to store the
OS image as well as the application and supporting
data files. To do this, complete the following sequence
of commands:
b. Copy the serial EEPROM setup script:
cp /tftp/159.97.84.210:setup.losh
/app/setup.losh
a. Erase the flash that the partition will exist in:
The expected output from this command is:
erase 0x00040000 0x01fc0000
cp /tftp/159.97.84.210:setup.losh ->
/app/setup.losh done
The expected output from this command is:
c. Copy the OS image:
unlocking flash blocks
erasing flash: 100%
erased '/dev/flash0' start=0x40000:
len=0x1fc0000 bytes
cp /tftp/159.97.84.210:nk.bin /app/nk.bin
51
5. Prior to upgrading the application, the IP address of the
ELSD must be determined. In step 15 of Section 7.5.1.3,
WinCE OS Initial Setup Procedure, the IP address of the
ELSD was recorded. Use this IP address. The rest of
this procedure assumes the ELSD was assigned the IP
address 159.97.84.10.
This command may take a minute to run. The expected
output from this command is:
cp /tftp/159.97.84.210:nk.bin -> /app/nk.bin
done
18. Next the serial EEPROM will be updated to mount the
YAFFS filesystem on power up and boot the OS. Run
the following command:
6. The ELSD will power up to a white screen.
7. Wait about 30 seconds before continuing. This gives
WinCE enough time to launch the OS and start the FTP
and telnet servers.
source /app/setup.losh
The expected output from this command is:
8.
# Setup serial EEPROM for booting from YAFFS
echo "LOLOadd-yaffs app nor 0x00040000
0x01fc0000; mount yaffs /app; cd /app;
source boot.losh; exit\r\n"
/dev/serial_eeprom
Next, establish an FTP connection to the ELSD. This
procedure assumes that Windows is being used to FTP
to the ELSD. Open ‘My Computer’ and type the
following into the address bar:
ftp://<IP>
Where <IP> is the IP address from step 5.
19. The OS image has been installed, the ELSD can be
rebooted.
20. Once the ELSD reboots, a white screen should appear.
The ELSD will appear to halt at this screen. This is
because no application is loaded yet; but WinCE
is running and the ELSD can be accessed with telnet
and FTP. Continue on to Section 7.5.1.4, Application
Initial Setup Procedure.
7.5.1.4 APPLICATION INITIAL SETUP PROCEDURE
The screen should look similar to the above.
Materials Needed:
•
•
•
9. Next, change to the app directory. There should be four
files listed in it. These are the initial boot files.
Crossover Ethernet cable
Application upgrade files
Tftpd32.exe software (installed on a pc)
1. Configure a standalone PC with static IP address. In this
example, an address of 159.97.84.210 will be used. It
doesn’t matter what address is used, but the rest of the
procedure will assume the above address.
NOTE: Make sure that this PC is not connected to any
other network. A DHCP server will be run on the
PC to assign an IP address to the ELSD. If this PC is
connected to a network that already has a DHCP server
running, both DHCP servers will be assigning addresses
to PC’s on the network. This will cause corrupting and
confusion on the network.
10. Next, the setup splash screen bitmap file will be
removed. This will be replaced by the application
splash screen. Select splash.bmp and delete it.
2. Connect the crossover Ethernet cable to the 3300 ELSD
and the PC.
11. Locate the folder where the ELSD application is stored:
3. Start running the Tftpd32.exe software. Make sure it is
configured the same as described in Section 7.5.1.3,
WinCE OS Initial Setup Procedure, steps 9 – 13.
4. Power up the 3300 ELSD.
52
16. Verify that the version numbers of the software
installed are correct. To display the version numbers,
go to the menu option: Maintenance/About.
17. The application upgrade procedure is complete. The
complete software installation procedure is also
complete.
12. Go into the application directory as shown in step 11.
13. Select all of the files and directories and drag them to
the FTP window from step 4. The copy should only
take a minute or so. Afterwards the FTP window should
look similar to:
14. Close the FTP connection to the ELSD.
15. Reboot the ELSD. The normal splash screen should
appear:
53
c. Contents inside the App folder on the pen drive (if
Application will be upgraded; otherwise, this folder would
be empty):
7.5.2 PEN DRIVE SOFTWARE UPGRADE PROCEDURE
The following procedure should be used to install new
application and/or OS software on the 3300 ELSD (when an
initial upgrade procedure isn’t necessary).
Materials Needed:
•
128MB (or less) USB pen drive loaded with new
software upgrade
NOTE: Pen drives with greater than 128MB are NOT
compatible with the 3300 ELSD.
1. First, confirm that the new software upgrade files have
been properly loaded onto the pen drive. The software
files should appear on the pen drive similar to the
following:
a. Main contents on the pen drive
d. Contents inside the OS folder on the pen drive (if OS will
be upgraded; otherwise, this folder would be empty):
2. Power off the 3300 ELSD.
b. Contents inside the Update folder on the pen drive
3. Insert the pen drive containing the upgrade files into the
USB Host port on the back panel of the 3300 ELSD.
4. Power up the 3300 ELSD.
5. The software installation should begin automatically.
Follow the instructions on the front panel as the
procedure continues. The screens should appear similar
to the following (software version numbers may differ):
a. In the first step, the update procedure determines if the
pen drive contains a new Application software version. If
so, the existing Application version and the new
Application version on the pen drive are displayed:
54
b. Press Yes to continue with the upgrade, and the update
procedure will continue on through the following steps:
e. Press Yes to continue on with the OS image upgrade. If
the existing OS version on the unit was 0.99.3 or above,
the upgrade will continue through the following steps. If
the existing OS version is below 0.99.3, then the update
procedure may involve a few extra steps, including a
reboot. In that case, follow the instructions on the screen
and press Yes or OK when indicated.
These steps may take several minutes to complete.
c. Once the Application update is completed, the following
screen will appear:
f. The pen drive upgrade procedure is complete. Power off
the 3300 ELSD and remove the pen drive.
g. Reboot the 3300 ELSD and confirm the new software
versions on the unit by selecting Maintenance/About.
d. Press OK and the update procedure will then determine
if the pen drive contains a new OS image upgrade. If so,
the following screen will appear that displays the existing
version on the unit and the new version on the pen drive.
If this is the first time a pen drive upgrade has been
performed on the unit, the existing version will be listed
as “Unknown”. This is normal.
55
7.6 CALIBRATION PROCEDURES
*These functions are available in Service Tech mode only.
NOTE: The detector must be in Standby mode in order to
be calibrated.
IMPORTANT: If the processor board has been replaced,
the serial number and date/time must be re-configured first
BEFORE the calibration procedures are performed.
Otherwise the calibration will not be saved. Refer to Section
3.4.2 for details on configuring the serial number, and refer
to Section 3.4.6 for details on configuring the date/time.
13. The left switch on the Temperature Calibration Box
o
should be set to 17 C. Press Continue and the next
screen in the calibration procedure will appear: Lower
Drift Tube Temp Calibration (High).
7.6.1 HEATER CALIBRATION
Tools Needed:
•
•
•
•
Anti-static strap
Phillips screwdriver
Temperature calibration box
Temperature probe (“Claw”) with thermometer
Reference: Section 7.7.1, Electronic Schematic
14. Flip the left switch to 96 °C. The Raw Value should
significantly increase. Press Continue to reach the next
step of the calibration:
Upper Drift Tube Temp
Calibration (Low).
Procedure:
1.
Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this calibration.
2.
Power off the unit from the back panel and disconnect
the power cord.
3.
Allow the unit to cool for at least 30 minutes.
4.
Using a Phillips screwdriver, remove the cover screws,
1 on each side and 4 on the back panel.
5.
Remove the ELSD cover by carefully sliding it toward
the back of the instrument.
6.
Disconnect the three RTDs (DT1, DT2, and Optics)
from the processor board (positions J22, J23, and J24
respectively).
7.
Connect the Temperature Calibration Box to the
processor board by connecting the left, middle, and
right cables to positions J22, J23, and J24 respectively.
8.
Set all three switches on the Temperature Calibration
Box to 17 °C.
9.
Power on the 3300 ELSD and wait for the instrument to
boot up.
o
15. The middle switch should be set to 17 C. Press
Continue to reach the next step of the calibration:
Upper Drift Tube Temp Calibration (High).
10. Select Maintenance/Service Tech/Enter Service Tech
Password using the arrows on the keypad and press
Enter.
16. Flip the middle switch to 96 °C. The Raw Value should
increase again. Press Continue to reach the next step
of the calibration: Optics Block Temp Calibration (Low).
11. Enter the password “atat” and press Accept to enter
Service Tech mode.
12. Select
Maintenance/Calibration/Heaters/Calibration
using the arrows on the keypad and press Enter. The
first screen of the heater calibration will then appear:
Lower Drift Tube Temp Calibration (Low)
56
25. If the measured temperatures are within tolerance
(±2°C at 40°C and 70°C and ±3°C at 100°C) then
heater calibration is finished. If any measured value is
not within tolerance, continue on to step 26.
26. Select
Maintenance/Calibration/Heaters/Correction
using the arrows on the keypad and press Enter to
reach the Temperature Correction screen:
o
17. The third switch should be set to 17 C. The raw value
should decrease. Press Continue to reach the next step of
the calibration: Optics Block Temp Calibration (High).
27. For the heated zones that are out of tolerance only,
enter the temperature values obtained in step 20, for
temperature set points of 40°C and 100°C. It is ok to
leave the blanks empty for the zones that are within
tolerance, but values must be entered for both
temperature set points for a given zone.
18. Flip the third switch to 96 °C. The Raw Value should
increase again. Press Continue to reach the final step
of the calibration.
28. Once the temperature values have been entered, press
Accept to modify the heater calibration.
29. Re-measure the temperatures of the heated zones
using the temperature probe and repeat the
Temperature Correction Procedure if necessary until
the heated zones are within tolerances.
19. Press Finish to complete the heater calibration and
return to the main screen.
20. To check the calibration, select Maintenance/Manual
Control and press Enter to reach the manual control
screen.
21. Flip each of the 3 toggle switches back and forth
between 17 °C and 96 °C and observe the values on
the screen. The temperatures should be 17 °C ± 0.2 °C
and 96°C ± 0.2 °C. If the temperature readings do not
meet the 17 °C ± 0.2 °C and 96 °C ± 0.2 °C
requirements, the unit must be recalibrated.
22. Press Accept to exit the Manual Control screen and
return to the main screen.
23. Replace the RTDs. Make sure they are installed in
order from top to bottom RTD 1, RTD 2, and RTD 3.
24. Physically check the temperatures using the
temperature probe (“claw”) in the three heater regions
and inside the drift tube at three set points, at 40°C,
70°C, and 100°C. When taking external temperature
measurements, make sure the temperature probe is in
direct contact with the copper tube and the heater.
Write down these temperature measurements.
57
7.6.2 GAS FLOW CALIBRATION
c. Enter a gas flow rate of 1.0L/min in the method, and
then press Accept.
Tools Needed:
d. Allow the instrument to stabilize, and watch the
output of the external flow meter. It should read
within ± 0.15 L/min of the set point.
•
•
•
•
•
Anti-static strap
Phillips screwdriver
External gas flow meter (Sierra 822S or equivalent)
1/2” open-end wrench
7/16” open-end wrench
e. Check the gas flow for the additional set points of 2.0,
3.0, and 4.0 L/min. If the unit is out of spec, repeat
the gas flow calibration.
f. Disconnect the external flow meter from the
instrument and re-connect the internal flow valve to
the internal flow meter.
Reference: Section 7.7.2, Gas Flow Path Schematic
Procedure:
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this calibration.
2. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
3. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set aside.
4. Connect the external flow meter in line between the
internal flow meter and the flow valve. Flow direction is
from meter to valve.
5. Connect a nitrogen gas line regulated to 80psi to the Gas
Inlet on the back panel of the 3300 ELSD.
6. Turn on the unit and wait for it to boot up.
7. Select Maintenance/Service Tech/Enter Service Tech
Password using the arrow keys, and press Enter.
8. Enter the password, “atat”, and press Accept.
9. Select Maintenance/Calibration/Gas Flow using the
arrows on the keypad, and then press Enter to reach the
first screen of the Gas Flow calibration procedure:
10. Allow the gas flow to equilibrate, and then take the
reading on the external flow meter. Enter the value into
the Observed Value box on the screen. The first reading
should be around 0.5 L/min. Then press Continue.
11. Repeat the same procedure for the next seven screens,
pressing Continue after each step is complete.
12. When the last step in the calibration is reached, press
Finish to finalize the calibration.
13. Check the calibration:
a. Select Operation/Mode/Run and then press Enter to
put the detector into Run mode.
b. Select Method/Edit and press Enter.
58
7.6.3 LASER/PREAMP CALIBRATION
Tools Needed:
•
•
•
•
•
•
•
Anti-static strap
Phillips screwdriver
Hex driver, 3/32”
Magnet
Preamp calibration fixture (including SMB cable)
Digital multimeter
Small screwdriver for adjusting potentiometers
d. Adjust the gain pot until a maximum voltage is
measured with the multimeter. (Laser is on.)
e. Press Continue to reach the next screen in the
laser/preamp calibration:
Procedure:
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this calibration.
2. Power off the unit from the back panel and disconnect
the power cord.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument.
f. Adjust the Offset pot until the multimeter reads 10mV.
(Laser is off.)
6. Use a 3/32 hex driver and a Phillips screwdriver to
remove the preamp and laser from the ELSD and install
both onto the calibration fixture.
g. Adjust the multimeter to read in Volts DC.
h. Press Continue to reach the next screen in
laser/preamp calibration:
7. Verify the calibration setup:
a. Laser is plugged into the processor board.
b. Preamplifier board is plugged into the processor
board.
c. Preamplifier ribbon cable is grounded.
d. SMB cable is connected to the preamplifier board.
e. SMB cable is connected to the voltmeter.
f. Voltmeter is set to read DC millivolts.
i. The target gain voltage is dependent on the fixture
being used. Adjust the Gain pot until it matches the
value listed on the fixture. (Laser is on.)
g. Magnet is on outside of chassis next to the magnetic
switch. (Do not center magnet on the switch. Place it
near one of the studs.)
j. Press Accept to reach the final step in the
laser/preamp calibration procedure:
h. Marked interlock on the instrument is replaced with
the fixture interlock.
i. Cover is installed on the preamp
8. Power on the instrument.
a. Using the arrow keys, navigate through the menus to
select Maintenance/Service Tech/Enter Service Tech
Password and hit Enter.
b. Enter the password “atat” and press Accept.
c. Select Maintenance/Calibration/Laser/Preamp and
press Enter. The first screen of the laser/preamp
calibration procedure will appear:
k. Press Finish to save the new laser/preamp
calibration.
l. Power off the instrument. Remove the magnet from
the chassis. Replace the interlock switch.
m. Reinstall the laser and preamp in the 3300 ELSD,
and replace the cover and screws.
59
FAN
HEATER
BOARD
SPEAKER
OPTICS
HEATER/
THERMOFUSES
UPPER DRIFT
TUBE HEATER/
THERMOFUSES
POWER
ENTRY
MODULE
OPTICS
RTD
POWER
SUPPLY
BOARD
UPPER DRIFT
TUBE RTD
LOWER DRIFT
TUBE RTD
PRESSURE
SENSOR
BATTERY
LOWER DRIFT
TUBE HEATER/
THERMOFUSES
POWER
INPUT
PRESSURE
SWITCH
7.7.1ELECTRONIC SCHEMATIC
7.7 SCHEMATICS
FLOW METER
ANALOG
SIGNAL
FPGA (J14)
CONNECTOR
GAIN
OFFSET
PRE-AMP
BOARD
RESET
BUTTON
CARD
ENGINE
SATELLITE
BOARD
MAGNETIC
INTERLOCK
SWITCHES
MEMBRANE
SWITCH
DISPLAY
BOARD
PROCESSOR
BOARD
FLOW VALVE
LCD INVERTER
INPUTS/
OUTPUTS
ETHERNET
USB DEVICE
USB HOST
RS232
LASER
63
DECIMAL: .XX ±.010"; .XXX ±.005"
FRACTIONAL: ± 1/64"
ANGULAR: ±1/2º
UNLESS OTHERWISE SPECIFIED
GENERAL TOLERANCES
This drawing is the property of Alltech
Associates, Inc. Any reproductions or
modifications of this drawing or its
contents without consent of Alltech is
prohibited.
CONFIDENTIAL:
LCD
SIGNAL OUTPUT
Alltech Associates, Inc.
2051 Waukegan Road, Deerfield, IL 60015
(847) 948-8600
MATERIAL:
DRAWN: WM
APPROVED: KC
SCALE: NTS DRAWING NO: SCHEMATIC
SIZE D
P/N:
DATE: 08/16/06
REV SHEET
1 OF 1
DESCRIPTION: 3300 ELECTRICAL SCHEMATIC/COMPONENTS
2
18
16
FLOW DIRECTION
SEE NOTE 2
4
SEE NOTE 1
1
3
4
14
20
10
11
NOTES:
1. APPLY PTFE TAPE TO ALL MALE NPT THREADS.
2. PLACE ITEMS 3, 5, AND 7 WITH THEIR RESPECTIVE ARROWS POINTING WITH THE DIRECTION OF THE FLOW.
19
12
7.7.2 GAS FLOW SCHEMATIC
7
6
FLOW DIRECTION
SEE NOTE 2
21
8
13
SEE NOTE 1
9
22
FLOW DIRECTION
SEE NOTE 2
5
15
SEE NOTE 1
Unequal Union 1/8 to 1/4 Tube - Push-In
Fitting
Gas Filter
Alltech Drawing
Number
Parker #
0003076 Scored Precision Orifice 1/8 Tube - 25u
Hole
0003072 Equall Tee 1/8 Tube - Push-In Fitting
0003083 Bulkhead Union 1/8 Tube - Push-In Fitting
0000838
0000838
0003096 3/16 OD X 3/32 ID X 13" L Vacuum Tube
0003404 Pressure Switch
0000838
0000838
0000838
0000838
0000838
0000838
10
11
12
13
14
15
16
17
18
19
20
21
22
DECIMAL: .XX ±.010"; .XXX ±.005"
FRACTIONAL: ± 1/64"
63
ANGULAR: ±1/2º
UNLESS OTHERWISE SPECIFIED
GENERAL TOLERANCES
This drawing is the property of Alltech
Associates, Inc. Any reproductions or
modifications of this drawing or its
contents without consent of Alltech is
prohibited.
CONFIDENTIAL:
1/8 OD X 1/16 ID X 5" L Tube
1/8 OD X 1/16 ID X 5" L Tube
1/8 OD X 1/16 ID X 6" L Tube
1/8 OD X 1/16 ID X 3.5" L Tube
1/8 OD X 1/16 ID X 4" L Tube
1/8 OD X 1/16 ID X 14" L Tube
1/8 OD X 1/16 ID X 12" L Tube
1/8 OD X 1/16 ID X 12" L Tube
*200-32
*200-32
*200-32
*200-32
*200-32
*200-32
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
2
1
2
1
1
1
Quantity
MATERIAL:
DRAWN: KS
APPROVED: WM
SCALE: 1 = 2 DRAWING NO:
0002889
SIZE C
P/N:
DATE: 09/14/06
REV SHEET
E 1 OF 1
2051 Waukegan Road, Deerfield, IL 60015
(847) 948-8600
-
-
-
-
-
-
-
-
-
-
-
-
A
-
-
A
-
A
-
-
-
D
Revision
Alltech Associates, Inc.
PS31-30-2MNB-A-S
P-FS40PSIR
EW-06409-16
*200-32
*200-32
0003083
364ML-2
0003076
AQ32-B-1
AQ52-P-2
0003229
W369ML-2-2
0003205
32PL-4-2
U-02909-10
377PL-2-2
0003207
Ref. #
DESCRIPTION: Gas Regulation System
Atlas Fibre #
Atlas Fibre #
Atlas Fibre #
Atlas Fibre #
Atlas Fibre #
Atlas Fibre #
Gems Sensors #
Atlas Fibre #
Atlas Fibre #
Atlas Fibre #
Parker #
Alkon #
Alkon #
0003074 1/16 Hose Barb to 1/8 Stem
9
Union Cross 1/8 Tube - Push-In Fitting
0003071
8
Alltech Drawing
Number
Parker #
Alltech Drawing
Number
Parker #
Cole Parmer P/N
0003229 Gas Flow Valve Cable Assembly
0003069 Male Elbow Swivel 1/8 NPT to 1/8 Tube Push-In Fitting
0003205 Gas Flow Meter Cable Assembly
0002981
Parker #
Alltech Drawing
Number
Ref. Type
7
6
5
4
0001873
0003068 Female Branch Swivel Tee 1/8 NPT to 1/8
Tube - Push-In Fitting
2
3
0003207 Pressure Switch Wiring Assembly
Title
1
Item
CM Part #
Number
17
7.8 HEATERS, RTDS, AND THERMOFUSES
7.8.1.2 CHECKING THE RTDS
7.8.1 CHECKING THE THERMOFUSES, RTDS, AND
HEATERS
Tools Needed:
7.8.1.1 CHECKING THE THERMOFUSES
•
•
•
Tools Needed:
•
•
•
Anti-static strap
Phillips screwdriver
Digital multimeter
Anti-static strap
Phillips screwdriver
Digital multimeter
Reference: Section 7.7.1, Electronic Schematic
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
Reference: Section 7.7.1, Electronic Schematic
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
2. Power off the unit from the back panel and disconnect the
power cord.
3. Before checking the thermofuses, first allow the resettable
fuses 2 hours to reset.
2. Power off the unit from the back panel and disconnect
the power cord.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
3. Before checking the thermofuses, first allow the
resettable fuses 2 hours to reset.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set aside.
4. Using a Phillips screwdriver, remove the cover screws,
1 on each side and 4 on the back panel.
6. Locate the connector(s) for the zones to be checked.
The connectors are located on the left side of the
processor board at positions J22, J23, and J24, which
correspond to lower drift tube, upper drift tube, and optics
block, respectively. Refer to Section 7.7.1, Electronic
Schematic for details.
5. Remove the ELSD cover by carefully sliding it toward
the back of the instrument and set aside.
6. Locate the connector(s) on the heater board for the
zones to be checked. The connectors are located at
positions J4, J5, and J6, which correspond to lower drift
tube, upper drift tube, and optics block, respectively.
Refer to Section 7.7.1, Electronic Schematic for details.
7. Disconnect the connector(s) from the Processor Board.
8. Using a multimeter, measure the resistance between the
wires. If there is infinite resistance, then the RTD needs
replacement. Refer to Section 7.8.2 for details on
replacing the RTD(s). If the RTD(s) are ok, then replace
the connectors back to their original positions, and
replace the 3300 ELSD cover and screws.
7. Disconnect the connector(s) from the Heater Board.
8. Using a multimeter, measure the resistance between
the thermofuse wires. The thermofuse wires are located
on the top row of each connector. If there is infinite
resistance between the wires, the thermofuse needs
replacement. Refer to Section 7.8.2.3, Thermofuse
Replacement Procedure, for details on replacing the
thermofuse(s). If the thermofuse(s) are ok, then replace
the connector(s) back to their original position(s), and
replace the 3300 ELSD cover and screws.
62
7.8.1.3 CHECKING THE HEATERS
7.8.2 HEATER, RTD, AND THERMOFUSE
REPLACEMENT PROCEDURES
Tools Needed:
•
•
•
7.8.2.1 HEATER REPLACEMENT PROCEDURE
Anti-static strap
Phillips screwdriver
Digital multimeter
Tools Needed:
•
•
•
•
•
•
Reference: Section 7.7.1, Electronic Schematic
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
Anti-static strap
Phillips screwdriver
Scissors
Replacement heater(s)
Kapton tape
Cable ties
Reference: Section 7.7.1, Electronic Schematic
2. Power off the unit from the back panel and disconnect the
power cord.
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
2. Power off the unit from the back panel and disconnect
the power cord.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument and set aside.
3. Allow the unit to cool for at least 30 minutes.
6. Locate the connector(s) on the heater board for the
zones to be checked. The connectors are located at
positions J4, J5, and J6, which correspond to lower drift
tube, upper drift tube, and optics block, respectively.
Refer to Section 7.7.1, Electronic Schematic for details.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
6. Disconnect the three connectors from the heater board
located at J4, J5, and J6. The heater wires for the drift
tube are labeled:
“Element 1” and “Element 2”
correspond to the lower drift tube heater zone; “Element
3” and “Element 4” correspond to the upper drift tube
heater zone. The third (unlabeled) connector contains
the wires for the optics block heaters.
7. Disconnect the connector(s) from the Heater Board.
8. Using a multimeter, measure the resistance between the
heater wires. The heater wires are located on the
bottom two rows of the connector. If there is infinite
resistance between the pair of wires in a row, then the
heater needs replacement. Refer to Section 7.8.2.1,
Heater Replacement Procedure, for details on replacing
the heater(s). If the heater(s) are ok, then replace the
connector(s) back to their original position(s), and
replace the 3300 ELSD cover and screws.
7. Cut the cable tie holding the heater wires by the heater
board.
8. Remove the drift tube insulation by finding the seam and
peeling it apart.
9. Loosen the drift tube end plates by removing six screws
to rotate the drift tube assembly as needed.
10. Cut the Kapton tape wrapped around the drift tube.
11. If replacing the drift tube heater continue on to step 12.
If replacing the optics block heaters proceed to step 17.
12. Peel off the RTD(s) from the drift tube.
13. Peel off the heater from the drift tube.
14. Remove the resettable fuses and thermofuses from the
drift tube.
15. Replace the drift tube heater assembly by peeling off
the protective film. Make sure the drift tube heater outer
surface is clean to ensure good adhesion. The wiring
for “Element 1” and “Element 2” should be towards the
front. Tape the drift tube heater to the drift tube at the
ends and middle with Kapton tape.
16. Tape the RTDs to the drift tube with Kapton tape.
17. Tape the resettable fuses and thermofuses to the drift
tube with Kapton tape.
63
7.8.2.2 RTD REPLACEMENT
18. If also replacing the optics block heaters continue on to
step 19. Otherwise, proceed to step 25.
Tools Needed:
19. Remove the retaining bracket screws located by the
drift tube outlet from the optics block.
•
•
•
•
•
•
20. Remove the clamp and screws holding the thermofuse
assembly underneath the optics block.
21. Remove the 2 existing cartridge heaters from the optics
block outer holes.
Anti-static strap
Phillips screwdriver
Scissors
Replacement RTD(s)
Kapton tape
Cable ties
22. Replace the optics heater assembly by installing 2 new
cartridge heaters back into the optics block outer holes.
Reference: Section 7.7.1, Electronic Schematic
23. Replace the retaining bracket with the two screws.
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
24. Replace the clamp and screws underneath the optics
block.
2. Power off the unit from the back panel and disconnect
the power cord.
25. Dress the heater wiring assembly against the drift tube
and tape it with Kapton tape.
3. Allow the unit to cool for at least 30 minutes.
26. Retighten the drift tube end plates with six screws.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
27. Reinstall the drift tube insulation making sure it adheres
to itself.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument.
28. Cable tie the heater wires by the heater board.
29. Reconnect the three wiring connectors to the heater
board.
6. Disconnect the three connectors from the processor
board located at J22, J23, and J24. Two of the
connectors are labeled: “1” corresponds to the lower drift
tube heater zone and “2” corresponds to the upper drift
tube heater zone. The third connector (unlabeled)
corresponds to the optics heater zone.
30. Replace the 3300 ELSD cover and screws.
7. Cut the cable ties holding the RTD wires.
8. Remove the drift tube insulation by finding the seam and
peeling it apart.
9. Loosen the drift tube end plates by removing the six
screws to rotate the drift tube assembly as needed.
10. Cut the Kapton tape wrapped around the drift tube.
11. If replacing the drift tube RTDs, continue on to step 12.
If only replacing the optics block RTDs, continue on to
step 13.
12. Peel off the existing RTD from the drift tube. Replace
with the new RTD by peeling off protective film and
adhering it to the drift tube. If also replacing the optics
block RTDs, continue on to step 13. Otherwise,
continue on to step 18.
13. Remove the retaining bracket and screws from the
optics block near the drift tube outlet.
14. Remove the existing RTD from the center hole on the
optics block.
15. Replace the new RTD by inserting it into the center hole
of the optics block.
16. Install the retaining bracket with two screws.
17. Dress the RTDs along the bracket and underneath the
bracket.
18. Reconnect the three RTD connectors to the processor
board making sure the RTD labeled 1 is at the top.
64
19. Tie the RTDs wiring with cable ties at the drift tube
outlet and the processor board bracket.
thermofuse, continue on to step 14; otherwise, continue
on to step 18.
14. Cut the two optics block thermofuse assembly wires from
the connector about two inches from the connector and
strip ends about 1/2”.
20. Retighten the drift tube end plates with six screws.
21. Reinstall the drift tube insulation making sure it adheres
to itself.
15. Remove the clamp and screws holding the assembly
underneath optics block.
22. Replace the 3300 ELSD cover and screws.
16. Replace the optics block thermofuse assembly by
stripping the wire ends about 1/2” and soldering them
together to the wires on the connector. Then install
shrink tubing over the solder points.
7.8.2.3 THERMOFUSE REPLACEMENT PROCEDURE
Tools Needed:
•
•
•
•
•
•
•
•
•
17. Install the clamp and screws underneath the optics
block.
Anti-static strap
Phillips screwdriver
Scissors
Replacement thermofuse(s)
Wire stripper
Soldering iron
Heat shrink tubing
Kapton tape
Cable ties
18. Dress the thermofuse wiring against the drift tube and
tape it with Kapton tape.
19. Tighten the drift tube end plates with the six screws.
20. Reinstall the drift tube insulation making sure it adheres
to itself.
21. Cable tie the heater wires by the heater board.
Reference: Section 7.7.1, Electronic Schematic
22. Reconnect the three wiring connectors to heater board.
1. Precaution must be taken (use of an anti-static foot
strap in a grounded environment) while performing
this procedure.
23.Replace the 3300 ELSD cover and screws.
2. Power off the unit from the back panel and disconnect
the power cord.
3. Allow the unit to cool for at least 30 minutes.
4. Using a Phillips screwdriver, remove the cover screws, 1
on each side and 4 on the back panel.
5. Remove the ELSD cover by carefully sliding it toward the
back of the instrument.
6. Disconnect the three wiring connectors from the heater
board located at J4, J5, and J6. The heater wires for the
drift tube are labeled: “Element 1” and “Element 2”
correspond to the lower drift tube heater zone; “Element
3” and “Element 4” correspond to the upper drift tube
heater zone. The third (unlabeled) connector contains
the wires for the optics block heated zone.
7. Cut the cable tie holding the wires by the heater board.
8. Remove the drift tube insulation by finding the seam and
peeling it apart.
9. Loosen the drift tube end plates by removing the six
screws to rotate the drift tube assembly as needed.
10. Cut the Kapton tape wrapped around the drift tube.
11. If replacing the drift tube thermofuse(s) continue on to
step 12. If only replacing the optics block thermofuse,
continue on to step 14.
12. Cut the two drift tube thermofuse assembly wires about
two inches from the connector and strip ends about 1/2”.
13. Replace the drift tube thermofuse assembly by stripping
the wire ends about 1/4” and soldering them together to
the wires on the connector. Then install shrink tubing
over the solder points. If also replacing the optics block
65
4. Measure the highest and lowest mV readings in each of
the three .2 minute intervals (2-2.2 min, 7-7.2 min and
12-12.2 min) in the 15-minute baseline trace to
determine the system noise. The average noise should
be less than or equal to 2 mV during the 15 minute
baseline trace.
7.9 MODEL 3300 ELSD QC PROCEDURE
Materials Needed:
• HPLC system with the ability to perform an accurate
and precise 20 µL injection
• HPLC grade Water and Acetonitrile, one liter premixed, H2O: ACN (45:55) for the mobile phase
• Hydrocortisone standard (Sigma, part number H4001)), stock solution of 1000µg/mL made in 100%
acetonitrile. Further dilutions made with HPLC grade
Water for a final concentration of 2 µg/mL.
• Alltech® Alltima™ C18, 5 µm, 250 x 4.6mm column
(Grace part number 88056)
• Universal Mini Filter, 1.2uL Internal Volume, Porosity
0.5um (Grace part number 77166) connected to
Liquid Inlet on detector
• Data collection device that can accept an analog
signal
Note: Due to the sensitivity of the detector, small random
spiking will occur. This is normal as long as the spikes are
included in the drift and noise measurements.
Procedure:
A. Sensitivity
1. Connect the Alltima™ C18 column between the injector
and detector. Make sure the 0.5um filter is connected to
the Liquid Inlet on the detector.
2. Program the ELSD 3300 to run with a drift tube
temperature set to 40ºC, gain set to 16, and the nitrogen
flow set to 1.5 L/min
3. Equilibrate the column with mobile phase for at least 1
hour.
4. Program the data station for an analysis of 5 minutes.
The only peak will be Hydrocortisone eluting at 3-3.5
minutes.
5. Make three 20µL injections of Hydrocortisone at a
concentration of 2 µg/mL.
6. Measure the noise for three 0.2 – 0.4 minute regions on
the baseline. Use the average noise value to calculate
the signal-to-noise ratio.
7. Calculate the average signal-to-noise-ratio from all three
injections. The average signal to noise ratio should be
equal to or greater than 15 with no more than two
random spikes larger than the noise per injection.
B. Drift and Noise Evaluation
1. Leave the Alltima™ C18 column in-line and continue
running the detector at the same conditions as in the
Sensitivity section (drift tube set to 40ºC, gas flow set to
1.5L/min, and gain set to 16) with mobile phase running
(55:45 acetonitrile:water at 1.0mL/min).
2. Collect a baseline trace for 15 minutes.
3. From this 15-minute baseline trace determine the
baseline drift by subtracting the lowest voltage reading
from the highest voltage reading. The baseline drift
should be less than or equal to 5mV.
66
7.10 VOLATILE MOBILE PHASE MODIFIERS
VOLATILE BUFFERS AND MOBILE PHASE MODIFIERS
Acids
Trifluoroacetic Acid
Formic Acid
Acetic Acid
Carbonic Acid
Bases
Ammonia
Methylamine
Ethylamine
Triethylamine
pKa
pKb
0.3
3.75
4.75
6.37
13.70
10.25
9.25
7.63
72.4°C
100.7°C
116.0°C
-
9.25
10.81
10.66
11.01
4.75
3.19
3.34
2.99
-33.35°C
16.6°C
-6.3°C
89.3°C
Buffers
Ammonium Formate
Pyridinium Formate
Ammonium Acetate
Pyridinium Acetate
Ammonium Carbonate
(used for reverse phase)
Ammonium Carbonate
Ion-Pair Reagents
Pentafluoropropionic Acid
Heptafluorobutyric Acid
Nonafluoropentanoic Acid
Pentadecafluorooctanoic Acid
Tridecafluoroheptanoic Acid
pH Range
BP
3.0-5.0
3.0-5.0
3.8-5.8
4.0-6.0
8.0 (adjusted)
120°C
111°C
5.5-7.5 and 9.3-11.3
~0.6
~0.6
~0.6
~0.6
~0.6
96-97°C
120°C
140°C
189°C
175°C
67
MP
7.11 WARRANTY, RETURNS, AND REPAIRS
SHIPMENTS
WARRANTY
All shipments are made F.O.B. Deerfield, IL.
Grace Davison Discovery Sciences warrants its products
against defects in workmanship or material under normal use
or service for one year. All obligations or liabilities under this
warranty are limited to repair or replacement, at Grace’s
option, F.O.B. Deerfield, IL, of parts that are returned, freight
prepaid and which are accepted as being defective upon
inspection by Grace.
DAMAGED SHIPMENTS
The Interstate Commerce Commission has held that carriers
are responsible for both concealed and visible damage
occurring during transit. Unpack the shipment upon receipt
and check for concealed damage even if no visible damage is
apparent. If concealed damage is discovered, stop unpacking
the unit, request an immediate inspection by the local carrier
agent, and obtain a written report of the findings to support a
claim. This request must be made within 15 days of receipt;
otherwise, the claim will not be honored by the carrier. Do not
return damaged goods to Grace without first obtaining an
inspection report and calling Grace for a Return Authorization
Number.
Components that are subject to normal wear and/or are
scheduled for routine replacement within the warranty period,
and/or parts, which are subjected to effects of corrosion or
deterioration by chemical or other action are excluded from the
above warranty for malfunction because of inadequate
facilities, operating conditions, or utilities.
Equipment and components may only be returned with
Grace’s prior approval and must bear a Grace Return
Authorization Number. Call the Grace Customer Service
Department to obtain a Return Authorization Number.
FILING OF CLAIMS
After a damage inspection report has been obtained, Grace
will cooperate in replacing damaged goods and in handling of
claims, which have been initiated by either party.
Guarantee/Warranties on accessories and equipment included
by Grace from other manufacturers are limited to the
guarantees given on such equipment by the respective
manufacturers.
RETURNS
If it is necessary to return any material to Grace, please call
Grace's Customer Service Department for a Return
Authorization Number and forwarding instructions. No returns
may be made without a Return Authorization Number.
Any modifications made to equipment covered by this
warranty, without written permission from Grace will void the
warranty. Grace reserves the right not to honor this warranty if
the products are obviously mishandled by the user.
REPAIRS
Grace is the only organization authorized to service or repair
the Model 3300 ELSD. Any repairs performed without
notifying Grace will void the warranty. To obtain repair
service, call Grace's Customer Service Department for
instructions and a Return for Repair Number.
Grace assumes no responsibility for consequential, economic
or incidental damages of any nature or on-site reinstallation
costs arising out of future alleged failure of any of its products
or their accessories.
This warranty supersedes any and all previous warranties
unless otherwise agreed upon at the time of sale, such as for
customized equipment.
68
7.12 USEFUL REFERENCES
CARBOHYDRATE APPLICATIONS
THEORY AND REVIEWS
Analysis of Carbohydrates using the Mass Detector, R.
Macrae and J. Dick, Journal of Chromatography, 210, 138145 (1981).
Evaporative Light Scattering Detection Solves Common
HPLC Detection Problems, M.J. Wilcox, International
Labmate, 23(6), 35-36 (1998).
High-Performance
Liquid
Chromatographic
Determination of Mono- and Oligosaccharides in Vegetables
with
Evaporative
Light-Scattering
Detection
and
Refractive Index Detection, J. Lopez Hernandez, M.J.
Gonzalez-Castro, I. Naya Alba, and C. de la Cruz Garcia,
Journal of Chromatographic Science, 36, 292-298 (1998).
Modified Laser Light-Scattering Detector for Use in High
Temperature Micro Liquid Chromatography, R. Trones, T.
Andersen, I. Hunnes, and T. Greibrokk, Journal of
Chromatography A, 814, 55-61 (1998).
GLYCERIDE, FATTY ACID, OIL APPLICATIONS
Improved Modification of Laser Light-Scattering Detector
for Use in Packed Capillary High Temperature Liquid
Chromatography, Roger Trones, Thomas Andersen, Tyge
Greibrokk, Journal of High Resolution Chromatography, 22(5),
283-286 (1999).
Determination of Nonvolatile Components of Heated
Soybean Oils Separated with High-Efficiency Mixed-Bed
Polystyrene/Divinylbenzene Columns, S.L. Abidi, I.H. Kim,
and K.A. Rennick, Journal of the American Oil Chemists'
Society, 76(8), 939-944 (1999).
The Evaporative Light-Scattering Detector, S. L. Hansen
and W.E. Artz, Inform, 6(2), 170-176 (1995).
Detect Anything Your LC Separates, P.A. Asmus, Research.
& Dev., 2, 96-98 (1993).
Non-Aqueous Reversed-Phase High-Performance Liquid
Chromatography of Synthetic Triacylglycerols and
Diacylglycerols, J-T Lin, C.L. Woodruff, and T.A. McKeon,
Journal of Chromatography A, 782, 41-48 (1997).
Evaporative Light Scattering Detectors for HPLC, GPC,
SEC, SFC - A Review, Bonnett, P.G., International LabMate,
15(5), 27-29 (1990).
Simulated Distillation of Heavy Oils Using an Evaporative
Light Scattering Detector, D.M. Padlo and E.L. Kugler,
Energy & Fuels, 10(5), 1031-1035 (1996).
Use of Light-Scattering as a Detector Principle in Liquid
Chromatography, A. Stolyhwo, H. Colin, G. Guiochon,
Journal of Chromatography, 265, 1-18 (1983).
Fast Monitoring of C20 – C160 Crude Oil Alkanes by SizeExclusion Chromatography-Evaporative Light Scattering
Detection Performed with Silica Columns, L. Carbognani,
Journal of Chromatography A, 788, 63-73 (1997).
A Light Scattering Detector for Liquid Chromatography,
P.B. Stockwell, B.W. King, American Laboratory, 19-24
(August 1991).
Analysis of Human Milk Triacylglycerols by HighPerformance Liquid Chromatography with LightScattering Detection, S.M. Pons, A.I. Castellote Bargallo,
and M.C. Lopez Sabater, Journal of Chromatography A, 823,
475-482 (1998).
Evaporative Analyzer as a Mass Detector for Liquid
Chromatography, John M. Charlesworth, Analytical
Chemistry, 50(11), 1414-1420 (September 1978).
Study of the Qualitative and Quantitative Properties of the
Light Scattering Detector, A. Stolyhwo, H. Colin, M. Martin,
G. Guiochon, Journal of Chromatography, 288, 253-275
(1984).
Evaluation by High-Performance Liquid Chromatography
of the Hydrolysis of Human Milk Triacylglycerides During
Storage at Low Temperatures, S.M. Pons, A.I. Castellote
Bargallo, and M.C. Lopez Sabater, Journal of Chromatography
A, 823, 467-474 (1998).
Influence of Various Parameters on the Response Factors
of the Evaporative Light Scattering Detector for a Number
of Non-Volatile Compounds, Georges Guiochon, Anne
Moysan,
Christopher
Holley,
Journal
of
Liquid
Chromatography, 11(12), 2547-2570 (1988).
Prediction of Relative Retention Times of Triacylglycerols
in Non-Aqueous Reversed-Phase High-Performance
Liquid Chromatography, J.-T. Lin, L.R. Snyder, and T.A.
McKeon, Journal of Chromatography A, 808, 43-49 (1998).
Analysis of Lipoxygenase Kinetics by High-Performance
Liquid Chromatography with a Polymer Column, A. Nunez
and G.J. Piazza, Lipids, 30(2), 129-133 (1995).
Effects of the Nature of the Solvent and Solutes on the
Response of a Light Scattering Detector, Michel Righezza,
Journal of Liquid Chromatography, 11(9 & 10), 1967-2004
(1988).
Gradient Reversed-Phase High-Performance Liquid
Chromatography
of
Saturated,
Unsaturated
and
Oxygenated Free Fatty Acids and Their Methyl Esters,
J.T. Lin, T.A. McKeon, and A.E. Stafford, Journal of
Chromatography A, 699, 85-91 (1995).
Effects of Wavelength of the Laser Beam on the Response
of an Evaporative Light Scattering Detector, Michel
Righezza, Journal of Liquid Chromatography, 11(13), 27092729 (1988).
69
Comparative High-Performance Liquid Chromatographic
Analyses of Cholesterol and Its Oxidation Products Using
Diode-Array Ultraviolet and Laser Light-Scattering
Detection, S. Kermasha, S. Kubow, and M. Goetghebeur,
Journal of Chromatography A, 685, 229-235 (1994).
Rapid Analysis of Oxidized Cholesterol Derivatives by
High-Performance Chromatography Combined with
Diode-Array Ultraviolet and Evaporative Laser LightScattering Detection, Kyoichi Osada, Amir Ravandi, and
Arns Kuksis, Journal of the American Oil Chemists' Society,
76(7), 863-871 (1999).
A Qualitative Method for Triglyceride Analysis by HPLC
Using an ELSD, W.S. Letter, Journal of Liquid
Chromatography, 16(1), 225-239 (1993).
Reversed-Phase
Separations
of
Nitrogenous
Phospholipids on an Octadecanoyl Poly (Vinyl Alcohol)
Phase, S.L. Abidi and T.L. Mounts, Journal of
Chromatography A, 773, 93-101 (1997).
Fatty Acid Composition of Human Milk Triglyceride
Species. Possible Consequences for Optimal Structures
of Infant Formula Triglycerides, Cheil H. Winter, Edda B.
Hoving, Frits A.J. Muskier, Journal of Chromatography, 616,
9-24 (1993).
Quantitative Analysis of Phosphatidylcholine Molecular
Species using HPLC and Light Scattering Detection, Jos
F.H.M. Brouwers, B.M. Gadella, L.M.G. van Golde, and
A.G.M. Tielens, Journal of Lipid Research, 39, 1-10 (1998).
Analysis of Triglycerides in Oils and Fats by Liquid
Chromatography with Laser Light-Scattering Detector,
Andrzej Stolywho, Henri Colin, Georges Guiochon, Analytical
Chemistry, 57, 1342-1354 (1985).
Quantitative High-Performance Liquid Chromatography
Analysis of Plant Phospholipids and Glycolipids Using
Light-Scattering Detection, G.A. Picchioni, A.E. Watada, and
B.D. Whitaker, Lipids, 31(2), 217-221 (1996).
Lipase G-Catalyzed Synthesis of Monoglycerides in
Organic Solvent and Analysis by HPLC, Casmir Akoh,
Carolyn Cooper, Chigozie Nwosu, Journal of the American Oil
Chemists’ Society, 69(9), (March 1992).
Separation of Synthetic Phosphatidylcholine Molecular
Species by High-Performance Liquid Chromatography on
a C8 Column, J-T Lin, C.L. Woodruff, T.A. McKeon, and J.A.
Singleton, Journal of Chromatography A, 824, 169-174 (1998).
Determination of the Positional Distribution of Fatty Acids
in Butter Fat Triacylglycerols, S. Kermasha, S. Kubow, M.
Safari, A. Reid, Journal of Chromatographic Science, 70, 169173 (1993).
New Procedures for Rapid Screening of Leaf Lipid
Components from Arabidopsis, W.W. Christie, S. Gill, J.
Nordback, Y. Itabashi, S. Sanda, and A.R. Slabas,
Phytochemical Analysis, 9, 53-57 (1998).
A New Variety of Low Linolenic Rapeseed Oil;
Characteristics and Room Odor Tests, A. Prevot, J.L. Perin,
G. Laclaverie, P.H. Auge, Coustille, J.L., Journal of the
American Oil Chemists’ Society, 67(3), 161 (March 1990).
Characterization of Rabbit Myocardial Phospholipase A2
Activity Using Endogenous Phospholipid Substrates, O.
Vesterqvist, C.A. Sargent, G.J. Grover, B. M. Warrack, G.C.
DiDonato, and M.L. Ogletree, Analytical Biochemistry, 217,
210-219 (1994).
Analysis of Tocopherols and Phytosterols in Vegetable
Oils by HPLC with Evaporative Light Scattering Detection,
K. Warner, T.L. Mounts, Journal of the American Oil Chemists’
Society, 67(11), (November 1990).
Separation of Lipid Classes from Plant Tissues by High
Performance Liquid Chromatography on Chemically
Bonded Stationary Phases, W.W. Christie and R.A. Urwin,
Journal of High Resolution Chromatography, 18, 97-100
(1995).
Analysis of Dimer Acids Using HPLC and the Evaporative
Light Scattering Detector, Peter Bonnett, Lipid Technology,
96-97 (July/August 1992).
Separation of Neutral Lipids by High-Performance Liquid
Chromatography:
Quantification by Ultraviolet, Light
Scattering and Fluorescence Detection, E. J. Murphy, T. A.
Rosenberger, and Lloyd A. Horrocks, Journal of
Chromatography B, 685, 9-14 (1996).
Comparison
of
Detectors
for
Size
Exclusion
Chromatography of Heavy Oil Related Samples, S.
Coulombe, Journal of Chromatographic Science, 26: 1-6
(1988).
LIPID APPLICATIONS
A Rapid Method for Phospholipid Separation by HPLC
Using a Light-Scattering Detector, W.S. Letter, Journal of
Liquid Chromatography, 15(2), 253-266 (1992).
Estimation of Free Glycolipids in Wheat Flour by HPLC,
J.B. Ohm, and O.K. Chung, Cereal Chemistry, 76(6), 873-876
(1999).
High Performance Liquid Chromatography of Lipids for
the Identification of Human Metabolic Disease, Thomas C.
Markello, Juanru Gu, and William A. Gahl, Analytic
Biochemist, 198, 368-374 (1991).
Fractionation of Soybean Phospholipids by HighPerformance Liquid Chromatography with an Evaporative
Light-Scattering Detector, Tong Wang, Earl G. Hammond,
James L. Cornette, and Walter R. Fehr, Journal of the
American Oil Chemists' Society, 76(11), 1313-1321 (1999).
Detection of HPLC Separation of Glycophospholipids:
Part 1, J.V. Amari, P.R. Brown, J.G. Turcotte, American
Laboratory , 23-29 (February 1992).
70
High-Throughput Characterization of Combinatorial
Libraries Generated by Parallel Synthesis, J.N. Kyranos
and J.C. Hogan, Analytical Chemistry, 70(1), 389A-395A
(1998).
Optimization of Detection for HPLC Separations of
Glycerophospholipids: Part 2, J.V. Amari, P.R. Brown, J.G.
Turcotte, American Laboratory, 26-33 (March 1992).
HPLC Analysis of Phospholipids by Evaporative Light
Scattering Detection, T.L. Mounts, S.L. Abidi, K.A. Rennick,
Journal of the American Oil Chemists’ Society, 69(5), 438-432
(May 1992).
Quantitation of Combinatorial Libraries of Small Organic
Molecules by Normal-Phase HPLC with Evaporative LightScattering Detection, C.E. Kibbey, Molecular Diversity, 1(4),
247-258 (1996).
High
Performance
Liquid
Chromatography
of
Phosphatidic Acids and Related Polar Lipids, S.L. Abidi,
Journal of Chromatography, 587, 193-203 (1991).
An Alternative Method for the Determination of Chloride in
Pharmaceutical Drug Substances Using HPLC and
Evaporative Light-Scattering Detection, D.S. Risley, J.A.
Peterson, K.L. Griffiths, and S. McCarthy, LC/GC, 14(12),
1040-1047 (1996).
An Improved Method for the Identification and
Quantitation of Biological Lipids by HPLC Using Laser
Light Scattering Detection, B.S. Lutzke, J.M. Braugler,
Journal of Lipid Research, 31, 2127-2130 (1990).
A High-Performance Liquid Chromatography Method for
the Quantitation of Impurities in an NMDA Antagonist
Using Evaporative Light Scattering Detection, D.S. Risley
and J.A. Peterson, Journal of Liquid Chromatography, 18(15),
3035-3048 (1995).
Rapid Separation and Quantification of Lipid Classes by
High Performance Liquid Chromatography and Mass
(Light Scattering) Detection, W.H. Christie, Journal of Lipid
Research, 26: 507-512 (1985).
Trace Analysis of a Weak UV-Absorbing Pharmaceutical
Compound in Swab Samples Using HPLC with
Evaporative Light-Scattering Detection, D.S. Risley, K.F.
Hostettler, and J.A. Peterson, LC/GC, 16(6),562-568 (1998).
Analysis of Neutral Lipids and Glycerolysis Products from
Olive Oil by Liquid Chromatography, Baokang Yang,
Jyhping Chen, Journal of the American Oil Chemist Society,
68(12), (December 1991).
POLYMER AND SURFACTANT APPLICATIONS
High-Performance Liquid Chromatographic Analysis of
Wheat Flour Lipids Using an Evaporative Light Scattering
Detector, F. Conforti, Carolyn H. Harris, Janet T. Rinehart,
Journal of Chromatography, 645, 83-88 (1993).
Universal Detection and Quantitation of Surfactants by
High-Performance Liquid Chromatography by Means of
the Evaporative Light-Scattering Detector, G.R. Bear,
Journal of Chromatography, 459, 91-107 (1988).
Determination of Cholesterol in Milk Fat by ReversedPhase High Performance Liquid Chromatography and
Evaporative Light Scattering Detection, George A. Spanos,
Steven J. Schwartz, LC/GC, 10(10), 774-777 (1992).
Chemical Characterization of Cellulose Acetate by NonExclusion Liquid Chromatography, T.R. Floyd, Journal of
Chromatography, 629, 243-254 (1993).
NUTRACEUTICAL/PHARMACEUTICAL
APPLICATIONS
Acrylic Block Copolymer Analysis by Adsorption
Chromatography with ELSD, B.L. Neff, H.J. Spinelli, Journal
of Applied Polymer Science, 42, 595-600 (1991).
Determination of Fumonisins B1, B2, B3, and B4 by HighPerformance Liquid Chromatography with Evaporative
Light-Scattering Detection, J.G. Wilkes, J.B. Sutherland, M.I.
Churchwell, and A.J. Williams, Journal of Chromatography A,
695, 319-323 (1995).
Use of an Evaporative Light Scattering Detector in
Reversed-Phase
High-Performance
Liquid
Chromatography of Oligomeric Surfactants, Y. Mengerink, H.C.
De Man, S.J. Van Der Wal, Journal of Chromatography, 552,
593-604 (1991).
High-Performance Liquid Chromatographic Analysis of
Ginseng Saponins Using Evaporative Light Scattering
Detection, M.K. Park, J.H. Park, S.B. Han, Y.G. Shin, and I.H.
Park, Journal of Chromatography A, 736, 77-81 (1996).
A Facile Separation of Nonactin and Its Homologues,
T. Herlt, Journal of Liquid Chromatography and Related
Technologies, 20(8), 1295-1300 (1997).
Simultaneous Resolution and Detection of a Drug
Substance, Impurities, and Counter Ion Using a MixedMode HPLC Column with Evaporative Light Scattering
Detection, M.D. Lantz, D.S. Risley, and J.A. Peterson, Journal
of Liquid Chromatography & Related Technologies, 20(9),
1409-1422 (1997).
71
MISCELLANEOUS APPLICATIONS
Newer Method for the Characterization of Higher
Molecular Mass Coal Derivatives, Keith D. Bartle, Erdol und
Kohle - Erdgas - Petrocheme Vereinigt mit Brennstoff, 36(1),
(January 1983).
Determination of the Mass Extractable in Organic
Solvents by Light Scattering Detection, Katherine S.
Hammond, Joanne Shatkin, Brian P. Leaderer, Applied
Occupational Environmental Hygiene, 7(1), 49-54 (January
1992).
Determination of Decyldimethyl Ammonium Chloride on
Wood Surfaces by HPLC with Evaporative Light
Scattering
Detection,
C.R.
Daniels,
Journal
of
Chromatographic Science, 30, 497-499 (December 1992).
ALLTECH® is a trademark, registered in the United States and/or other countries, of Alltech Associates, Inc. SOFGRIP™ is a trademark of Alltech Associates, Inc.
GRACE® and GRACE DAVISON® are trademarks, registered in the United States and/or other countries, of W. R. Grace & Co.-Conn. GRACE DAVISON
DISCOVERY SCIENCES™ is a trademark of W. R. Grace & Co.-Conn. WINDOWS® is a trademark of Microsoft Corporation.
This trademark list has been compiled using available published information as of the publication date of this brochure and may not accurately reflect
current trademark ownership.
Grace Davison Discovery Sciences is a product group of W. R. Grace & Co.-Conn. Alltech Associates, Inc. is a wholly owned subsidiary of W. R. Grace & Co.-Conn.
© Copyright 2007 Alltech Associates, Inc. All rights reserved.
72
www.discoverysciences.com
Grace Davison Discovery Sciences Regional Headquarters
In the Americas
2051 Waukegan Road • Deerfield, Illinois 60015-1899
Tel: 847.948.8600 • Fax: 847.948.1078
Email: [email protected]
Web: www.discoverysciences.com
In Europe
Brandstraat 12 • B-9160 Lokeren, Belgium
Tel: +32 (0)9 340 65 65 • Fax: +32 (0)9 340 65 60
Email: [email protected]
Web: www.discoverysciences.com/be
In Asia
19th Floor • K. Wah Center • 1010 Hua Hai Zhong Road
Shanghai 200031, P.R.C.
Tel: 86 21 54674678 • Fax: 86 21 54051500
Email: [email protected]
Web: www.discoverysciences.com/cn
In Australia
30 Brookhollow Avenue • Baulkham Hills
New South Wales 2153, Australia
Tel: 1300 36 24 12 • Fax: 1300 36 24 11
Email: [email protected]
Web: www.discoverysciences.com/au
73